Annulated carbocyclic gallylene and bis-gallylene with two-coordinated Ga(i) atoms.
Merschel, Arne; Heda, Shkelqim; Vishnevskiy, Yury V.; Neumann, Beate; Stammler, Hans-Georg; Ghadwal, Rajendra S.; Chemical science 16 (2025) 2222–2230; doi:10.1039/d4sc06782g

data_1573161
_publ_section_title
;
 Annulated carbocyclic gallylene and bis-gallylene with two-coordinated
 Ga(i) atoms.
;
_journal_issue                   5
_journal_name_full               'Chemical science'
_journal_page_first              2222
_journal_page_last               2230
_journal_paper_doi               10.1039/d4sc06782g
_journal_volume                  16
_journal_year                    2025
_chemical_formula_moiety         '2(C40 H39 F8 Ga N2)'
_chemical_formula_sum            'C80 H78 F16 Ga2 N4'
_chemical_formula_weight         1538.90
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2023-12-14
_audit_creation_method
;
Olex2 1.5-alpha
(compiled 2023.11.24 svn.r209d9fb2 for OlexSys, GUI svn.r6869)
;
_audit_update_record
;
2024-02-23 deposited with the CCDC.	2024-11-14 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 100.679(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.4377(4)
_cell_length_b                   19.6182(4)
_cell_length_c                   19.7964(5)
_cell_measurement_reflns_used    8184
_cell_measurement_temperature    100.0(1)
_cell_measurement_theta_max      71.8690
_cell_measurement_theta_min      3.1780
_cell_volume                     7418.3(3)
_computing_cell_refinement       'CrysAlisPro 1.171.43.93a (Rigaku OD, 2023)'
_computing_data_collection
'CrysAlisPro system (CCD 43.93a 64-bit (release 17-10-2023))'
_computing_data_reduction        'CrysAlisPro 1.171.43.93a (Rigaku OD, 2023)'
_computing_molecular_graphics    'Olex2 1.5-alpha (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-alpha (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      100.0(1)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.3114
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.965
_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    -55.00  -6.00   1.00   40.00    --  -38.50 125.00 -30.00   49
  2  \w   -107.00 -21.00   1.00   40.00    --  -38.50 -57.00 120.00   86
  3  \w     18.00  73.00   1.00   40.00    --   42.95  57.00 -90.00   55
  4  \w     30.00  58.00   1.00   40.00    --   42.95-125.00  30.00   28
  5  \w    113.00 156.00   1.00  110.00    --  101.85 125.00-180.00   43
  6  \w     34.00 112.00   1.00  110.00    --  101.85-125.00 -30.00   78
  7  \w     62.00 172.00   1.00  110.00    --  101.85  15.00-150.00  110
  8  \w     97.00 141.00   1.00  110.00    --  101.85 125.00  90.00   44
  9  \w     79.00 171.00   1.00  110.00    --  101.85  45.00 -90.00   92
 10  \w    110.00 168.00   1.00  110.00    --  101.85 125.00 120.00   58
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0516660000
_diffrn_orient_matrix_UB_12      -0.0565727000
_diffrn_orient_matrix_UB_13      -0.0111714000
_diffrn_orient_matrix_UB_21      0.0163526000
_diffrn_orient_matrix_UB_22      0.0384577000
_diffrn_orient_matrix_UB_23      -0.0630556000
_diffrn_orient_matrix_UB_31      0.0597705000
_diffrn_orient_matrix_UB_32      0.0384407000
_diffrn_orient_matrix_UB_33      0.0466209000
_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  0.0450
_diffrn_reflns_av_unetI/netI     0.0618
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.965
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            29275
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.965
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         71.879
_diffrn_reflns_theta_min         3.199
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.633
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.824
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.43.93a (Rigaku Oxford Diffraction, 2023)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.378
_exptl_crystal_description       prism
_exptl_crystal_F_000             3168
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.668
_refine_diff_density_min         -0.471
_refine_diff_density_rms         0.079
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     935
_refine_ls_number_reflns         14048
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.0728
_refine_ls_R_factor_gt           0.0522
_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^)+(0.0604P)^2^+6.4108P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1232
_refine_ls_wR_factor_ref         0.1350
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10814
_reflns_number_total             14048
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4sc06782g2.cif
_cod_data_source_block           11
_cod_depositor_comments
'Adding full bibliography for 1573160--1573166.cif.'
_cod_database_code               1573161
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C80H78F16Ga2N4
_chemical_oxdiff_usercomment     'Mounted by Arne'
_shelx_estimated_absorpt_t_max   0.908
_shelx_estimated_absorpt_t_min   0.747
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C23(H23), C35(H35), C78(H78), C66(H66), C26(H26), C75(H75), C63(H63), C38(H38)
2.b Aromatic/amide H refined with riding coordinates:
 C16(H16), C73(H73), C56(H56), C52(H52), C12(H12), C54(H54), C53(H53),
 C61(H61), C14(H14), C13(H13), C15(H15), C31(H31), C59(H59), C72(H72), C71(H71),
  C19(H19), C33(H33), C60(H60), C55(H55), C32(H32), C21(H21), C20(H20)
2.c Idealised Me refined as rotating group:
 C37(H37A,H37B,H37C), C67(H67A,H67B,H67C), C24(H24A,H24B,H24C), C76(H76A,H76B,
 H76C), C27(H27A,H27B,H27C), C64(H64A,H64B,H64C), C25(H25A,H25B,H25C), C80(H80A,
 H80B,H80C), C68(H68A,H68B,H68C), C79(H79A,H79B,H79C), C77(H77A,H77B,H77C),
 C36(H36A,H36B,H36C), C28(H28A,H28B,H28C), C65(H65A,H65B,H65C), C39(H39A,H39B,
 H39C), C40(H40A,H40B,H40C)
;
_shelx_res_checksum              63906
_shelx_hkl_checksum              85927
_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 2.181
_oxdiff_exptl_absorpt_empirical_full_min 0.594