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_1573160
_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_absolute_configuration ad
_chemical_formula_moiety         'C66 H82 Ga2 N4, 3(C6 H6)'
_chemical_formula_sum            'C84 H100 Ga2 N4'
_chemical_formula_weight         1305.11
_space_group_crystal_system      tetragonal
_space_group_IT_number           110
_space_group_name_Hall           'I 4bw -2c'
_space_group_name_H-M_alt        'I 41 c d'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2022-02-21
_audit_creation_method
;
Olex2 1.3-ac4
(compiled 2019.04.23 svn.r3594 for Rigaku Oxford Diffraction, GUI svn.r5739)
;
_audit_update_record
;
2024-02-23 deposited with the CCDC.	2024-11-14 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   17.2516(2)
_cell_length_b                   17.2516(2)
_cell_length_c                   47.4743(8)
_cell_measurement_reflns_used    51064
_cell_measurement_temperature    100.0(1)
_cell_measurement_theta_max      28.8630
_cell_measurement_theta_min      2.6490
_cell_volume                     14129.2(3)
_computing_cell_refinement       'CrysAlisPro 1.171.41.122a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.122a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.122a (Rigaku OD, 2021)'
_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_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 0.999
_diffrn_measured_fraction_theta_max 0.999
_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    -41.00   0.25   0.75   32.00    --  -17.24 -77.00 150.00   55
  2  \w    -47.00 -20.00   0.75   32.00    --  -17.24  77.00-180.00   36
  3  \w    -21.00   5.25   0.75   32.00    --  -17.24 -77.00 -90.00   35
  4  \w    -42.00   5.25   0.75   32.00    --  -17.24 -77.00  90.00   63
  5  \w     40.00  88.00   0.75   32.00    --   17.24 178.00 -60.00   64
  6  \w     58.00  99.25   0.75   32.00    --   17.24-178.00  90.00   55
  7  \w    -75.00 -45.00   0.75   64.00    --  -17.08 131.00-135.25   40
  8  \w    -91.00 -64.75   0.75   64.00    --  -17.08 154.00 -56.12   35
  9  \w     -4.00  87.50   0.75   64.00    --   17.08  38.00  90.00  122
 10  \w    -49.00  37.25   0.75   64.00    --   17.08 -38.00 -90.00  115
 11  \w    -28.00  52.25   0.75   64.00    --   17.08 -90.00 162.91  107
 12  \w    -46.50  42.00   0.75   64.00    --   17.08 -57.00  60.00  118
 13  \w     -1.00  90.50   0.75   64.00    --   17.08  29.00-119.00  122
 14  \w     -8.00  85.00   0.75   64.00    --   17.08  57.00 -30.00  124
 15  \w    -72.00 -29.25   0.75   64.00    --  -17.08 126.00 149.47   57
 16  \w    -91.00 -43.00   0.75   64.00    --  -17.08 154.00-116.63   64
 17  \w    -42.00  12.00   0.75   64.00    --  -17.08 -77.00 -60.00   72
 18  \w    -42.00  12.00   0.75   64.00    --  -17.08 -77.00-180.00   72
 19  \w    -90.00 -42.00   0.75   64.00    --  -17.08 153.00  47.92   64
 20  \w    -72.00 -29.25   0.75   64.00    --  -17.08 126.00  17.15   57
 21  \w     16.00  68.50   0.75   64.00    --   17.08-147.00  53.43   70
;
_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      -0.0042341000
_diffrn_orient_matrix_UB_12      0.0383139000
_diffrn_orient_matrix_UB_13      0.0051967000
_diffrn_orient_matrix_UB_21      -0.0406860000
_diffrn_orient_matrix_UB_22      -0.0025384000
_diffrn_orient_matrix_UB_23      -0.0019052000
_diffrn_orient_matrix_UB_31      -0.0039900000
_diffrn_orient_matrix_UB_32      -0.0147082000
_diffrn_orient_matrix_UB_33      0.0138811000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0863
_diffrn_reflns_av_unetI/netI     0.0288
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       66
_diffrn_reflns_limit_l_min       -66
_diffrn_reflns_number            222973
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.029
_diffrn_reflns_theta_min         2.675
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.810
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.77703
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.122a (Rigaku Oxford Diffraction, 2021)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.227
_exptl_crystal_description       plate
_exptl_crystal_F_000             5552
_exptl_crystal_size_max          0.07
_exptl_crystal_size_mid          0.069
_exptl_crystal_size_min          0.026
_refine_diff_density_max         0.370
_refine_diff_density_min         -0.262
_refine_diff_density_rms         0.056
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.484(11)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.109
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     426
_refine_ls_number_reflns         10335
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.109
_refine_ls_R_factor_all          0.0442
_refine_ls_R_factor_gt           0.0336
_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^)+(0.0372P)^2^+10.5949P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0780
_refine_ls_wR_factor_ref         0.0826
_reflns_Friedel_coverage         0.977
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.999
_reflns_number_gt                9117
_reflns_number_total             10335
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4sc06782g2.cif
_cod_data_source_block           3x2C6H6
_cod_depositor_comments
'Adding full bibliography for 1573160--1573166.cif.'
_cod_original_cell_volume        14129.1(4)
_cod_database_code               1573160
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C78 H104 Ga2 N2'
_shelx_estimated_absorpt_t_max   0.979
_shelx_estimated_absorpt_t_min   0.945
_reflns_odcompleteness_completeness 99.83
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     29.97
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.516(11)
 0.484(11)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3.a Ternary CH refined with riding coordinates:
 C15(H15), C18(H18), C31(H31), C34(H34)
3.b Aromatic/amide H refined with riding coordinates:
 C6(H6), C7(H7), C8(H8), C11(H11), C12(H12), C13(H13), C22(H22), C23(H23),
 C24(H24), C27(H27), C28(H28), C29(H29), C37(H37), C38(H38), C39(H39), C40(H40),
  C41(H41), C42(H42), C43(H43), C44(H44), C45(H45)
3.c Idealised Me refined as rotating group:
 C16(H16A,H16B,H16C), C17(H17A,H17B,H17C), C19(H19A,H19B,H19C), C20(H20A,H20B,
 H20C), C32(H32A,H32B,H32C), C33(H33A,H33B,H33C), C35(H35A,H35B,H35C), C36(H36A,
 H36B,H36C)
;
_shelx_res_checksum              88140
_shelx_hkl_checksum              5123
_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 1.299
_oxdiff_exptl_absorpt_empirical_full_min 0.892