Metal-metal cooperativity boosts Lewis basicity and reduction properties of the bis(gallanediyl) <sup>Cy</sup>L<sub>2</sub>Ga<sub>2</sub>.
Helling, Christoph; Döhler, Lotta; Kysliak, Oleksandr; Görls, Helmar; Liebing, Phil; Wölper, Christoph; Kretschmer, Robert; Schulz, Stephan; Dalton transactions (Cambridge, England : 2003) 53 (2024) 4922–4929; doi:10.1039/d4dt00172a

data_7715242
_publ_section_title
;
 Metal-metal cooperativity boosts Lewis basicity and reduction properties
 of the bis(gallanediyl) <sup>Cy</sup>L<sub>2</sub>Ga<sub>2</sub>.
;
_journal_issue                   11
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              4922
_journal_page_last               4929
_journal_paper_doi               10.1039/d4dt00172a
_journal_volume                  53
_journal_year                    2024
_chemical_absolute_configuration unk
_chemical_formula_moiety         'C38 H65 Ga N4 O2'
_chemical_formula_sum            'C38 H65 Ga N4 O2'
_chemical_formula_weight         679.66
_space_group_crystal_system      monoclinic
_space_group_IT_number           5
_space_group_name_Hall           'C 2y'
_space_group_name_H-M_alt        'C 1 2 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2021-11-12
_audit_creation_method
;
Olex2 1.3
(compiled Nov 21 2019 18:26:39 for OlexSys, GUI svn.r6003)
;
_audit_update_record
;
2022-01-04 deposited with the CCDC.	2024-02-14 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 108.583(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   20.896(3)
_cell_length_b                   11.1691(13)
_cell_length_c                   16.8820(19)
_cell_measurement_reflns_used    9893
_cell_measurement_temperature    120
_cell_measurement_theta_max      32.27
_cell_measurement_theta_min      2.27
_cell_volume                     3734.7(8)
_computing_cell_refinement       'SAINT V8.40B (Bruker, 2016)'
_computing_data_collection       'SAINT V8.40B (Bruker, 2016)'
_computing_data_reduction        'SAINT V8.40B (Bruker, 2016)'
_computing_molecular_graphics    'Diamond 4 (Brandenburg, 1997)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      120
_diffrn_detector                 'Bruker APEX II'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker-Nonius Kappa-CCD'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0782
_diffrn_reflns_av_unetI/netI     0.0898
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            26209
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.999
_diffrn_reflns_theta_min         2.045
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_current           0.6
_diffrn_source_power             0.03
_diffrn_source_type              'Incoatec I\ms'
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.773
_exptl_absorpt_correction_T_max  0.746591
_exptl_absorpt_correction_T_min  0.435768
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 TWINABS-2012/1 (Bruker,2012) was used for absorption correction.

Final HKLF 4 output contains 60469 reflections, Rint = 0.0782
 (19222 with I > 3sig(I), Rint = 0.0670)
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.209
_exptl_crystal_description       prism
_exptl_crystal_F_000             1472
_exptl_crystal_size_max          0.46
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.12
_refine_diff_density_max         4.223
_refine_diff_density_min         -1.558
_refine_diff_density_rms         0.139
_refine_ls_abs_structure_details
;
 Flack x determined using 4140 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.313(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     462
_refine_ls_number_reflns         26209
_refine_ls_number_restraints     25
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.0831
_refine_ls_R_factor_gt           0.0810
_refine_ls_shift/su_max          0.011
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1542P)^2^+4.6867P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2017
_refine_ls_wR_factor_ref         0.2049
_reflns_Friedel_coverage         0.905
_reflns_Friedel_fraction_full    0.998
_reflns_Friedel_fraction_max     0.993
_reflns_number_gt                25273
_reflns_number_total             26209
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt00172a2.cif
_cod_data_source_block           bn00066_tw4
_cod_depositor_comments
'Adding full bibliography for 7715237--7715242.cif.'
_cod_original_cell_volume        3734.6(8)
_cod_database_code               7715242
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.913
_shelx_estimated_absorpt_t_min   0.717
_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. Shared sites
{C18A, C18B}
{C19A, C19B}
3. Restrained distances
 C18A-C20A \\sim C18A-C20B
 with sigma of 0.005
4. Uiso/Uaniso restraints and constraints
C16A \\sim C17A: within 2A with sigma of 0.001 and sigma for terminal atoms of
0.002 within 2A
C16B \\sim C17B: within 2A with sigma of 0.001 and sigma for terminal atoms of
0.002 within 2A
C20A \\sim C20B: within 2A with sigma of 0.005 and sigma for terminal atoms of
0.01 within 2A
Uanis(C15B) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(C20A) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(C20B) \\sim Ueq: with sigma of 0.003 and sigma for terminal atoms of 0.006
Uanis(C18A) = Uanis(C18B)
Uanis(C19A) = Uanis(C19B)
5. Others
 Sof(C15B)=Sof(H15B)=Sof(C16B)=Sof(H16D)=Sof(H16E)=Sof(H16F)=Sof(C17B)=
 Sof(H17D)=Sof(H17E)=Sof(H17F)=1-FVAR(1)
 Sof(C15A)=Sof(H15A)=Sof(C16A)=Sof(H16A)=Sof(H16B)=Sof(H16C)=Sof(C17A)=
 Sof(H17A)=Sof(H17B)=Sof(H17C)=FVAR(1)
 Sof(C20B)=Sof(H20D)=Sof(H20E)=Sof(H20F)=Sof(C18B)=Sof(H18B)=Sof(C19B)=
 Sof(H19D)=Sof(H19E)=Sof(H19F)=1-FVAR(2)
 Sof(C20A)=Sof(H20A)=Sof(H20B)=Sof(H20C)=Sof(C18A)=Sof(H18A)=Sof(C19A)=
 Sof(H19A)=Sof(H19B)=Sof(H19C)=FVAR(2)
6.a Ternary CH refined with riding coordinates:
 C1(H1), C15A(H15A), C18A(H18A), C15B(H15B), C18B(H18B)
6.b Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C3(H3A,H3B), C22(H22A,H22B), C23(H23A,H23B), C24(H24A,H24B),
 C31(H31A,H31B), C32(H32A,H32B), C33(H33A,H33B)
6.c Aromatic/amide H refined with riding coordinates:
 C6(H6), C11(H11), C12(H12), C13(H13)
6.d Idealised Me refined as rotating group:
 C4(H4A,H4B,H4C), C8(H8A,H8B,H8C), C26(H26A,H26B,H26C), C27(H27A,H27B,H27C),
 C28(H28A,H28B,H28C), C29(H29A,H29B,H29C), C35(H35A,H35B,H35C), C36(H36A,H36B,
 H36C), C37(H37A,H37B,H37C), C38(H38A,H38B,H38C), C20A(H20A,H20B,H20C),
 C16A(H16A,H16B,H16C), C17A(H17A,H17B,H17C), C19A(H19A,H19B,H19C), C20B(H20D,
 H20E,H20F), C16B(H16D,H16E,H16F), C17B(H17D,H17E,H17F), C19B(H19D,H19E,H19F)
;
_shelx_res_checksum              54557
_olex2_date_sample_data_collection 2021-11-11
_olex2_date_sample_submission    2021-11-01
_olex2_submission_original_sample_id OK-G140
_olex2_submission_special_instructions 'No special instructions were received'