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_1573165
_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         'C66 H78 Ga2 I4 N4'
_chemical_formula_sum            'C66 H78 Ga2 I4 N4'
_chemical_formula_weight         1574.446
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_Int_Tables_number      2
_atom_sites_solution_primary     dual
_audit_creation_date             2023-05-03
_audit_creation_method
;
Olex2 1.5-dev
(compiled 2023.04.26 svn.r751481ca for OlexSys, GUI svn.r6777)
;
_audit_update_record
;
2024-02-23 deposited with the CCDC.	2024-11-14 downloaded from the CCDC.
;
_cell_angle_alpha                101.963(1)
_cell_angle_beta                 98.911(1)
_cell_angle_gamma                107.530(1)
_cell_formula_units_Z            1
_cell_length_a                   10.5694(1)
_cell_length_b                   12.1801(1)
_cell_length_c                   13.6704(1)
_cell_measurement_reflns_used    91448
_cell_measurement_temperature    100.0(1)
_cell_measurement_theta_max      37.4340
_cell_measurement_theta_min      3.5580
_cell_volume                     1596.52(3)
_computing_cell_refinement       'CrysAlisPro 1.171.42.88a (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.42.88a (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.42.88a (Rigaku OD, 2023)'
_computing_molecular_graphics    'Olex2 1.5-dev (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-dev (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine 1.5-dev (Bourhis et al., 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100.0(1)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.1773
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.9978
_diffrn_measured_fraction_theta_max 0.9687
_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    -53.00   2.00   1.00    7.50    --   -9.78 108.00  23.00   55
  2  \w     -8.00  53.00   1.00    7.50    --   10.17-108.00 -73.00   61
  3  \w    -79.00 -18.00   1.00    7.50    --   -9.78 147.00  58.56   61
  4  \w    -84.00 -59.00   1.00    7.50    --   -9.78 153.00 -69.34   25
  5  \w    -41.00  42.00   1.00    7.50    --   -9.78  77.00 -60.00   83
  6  \w    -12.00  67.00   1.00    7.50    --   10.17  38.00-120.00   79
  7  \w     -4.00  42.00   1.00    7.50    --   10.17  77.00-180.00   46
  8  \w     21.00  47.00   1.00    7.50    --   10.17-154.00 -73.00   26
  9  \w     -8.00  67.00   1.00    7.50    --   10.17  38.00 -60.00   75
 10  \w     60.00  85.00   1.00    7.50    --   10.17-154.00 -73.00   25
 11  \w      2.00  83.00   1.00    7.50    --   10.17  38.00   0.00   81
 12  \w    -16.00  79.00   1.00    7.50    --   10.17  57.00  90.00   95
 13  \w     -6.00  71.00   1.00   10.00    --   30.16-108.00 -73.00   77
 14  \w    -56.00  39.00   1.00   10.00    --  -29.85  57.00  60.00   95
 15  \w    -20.00   8.00   1.00   10.00    --  -29.85 -95.00  30.62   28
 16  \w   -105.00 -73.00   1.00   10.00    --  -29.85 -19.00 -30.00   32
 17  \w    -99.00 -19.00   1.00   10.00    --  -29.85 147.00-121.58   80
 18  \w    -67.00 -10.00   1.00   10.00    --  -29.85 -19.00 -30.00   57
 19  \w    -14.00  12.00   1.00   10.00    --  -29.85-104.00 175.91   26
 20  \w     -8.00  18.00   1.00   10.00    --   30.16  97.00 -29.22   26
 21  \w     12.00 103.00   1.00   10.00    --   30.16  38.00 -30.00   91
 22  \w     19.00  99.00   1.00   10.00    --   30.16-146.00-174.61   80
 23  \w      8.00 100.00   1.00   10.00    --   30.16  38.00 150.00   92
 24  \w      8.00 100.00   1.00   10.00    --   30.16  38.00-120.00   92
 25  \w     -7.00  19.00   1.00   10.00    --   30.16  96.00 160.72   26
 26  \w     40.00 116.00   1.00   10.00    --   30.16 178.00 -90.00   76
 27  \w     10.00  96.00   1.00   10.00    --   30.16  57.00  30.00   86
 28  \w     -8.00  18.00   1.00   10.00    --   30.16-108.00 -73.00   26
 29  \w     46.00  72.00   1.00   10.00    --   30.16-108.00 -73.00   26
 30  \w    -56.00  40.00   1.00   10.00    --  -29.85  57.00  60.00   96
 31  \w   -100.00  -3.00   1.00   10.00    --  -29.85 -57.00 -30.00   97
 32  \w   -108.00 -15.00   1.00   10.00    --  -29.85 -19.00 -30.00   93
 33  \w   -100.00  -3.00   1.00   10.00    --  -29.85 -57.00  60.00   97
 34  \w    -73.00   8.00   1.00   10.00    --  -29.85 108.00  23.00   81
 35  \w     39.00 117.00   1.00   10.00    --   30.16 178.00-180.00   78
 36  \w     39.00 117.00   1.00   10.00    --   30.16 178.00 -60.00   78
 37  \w    -15.00  69.00   1.00   10.00    --   30.16 -99.00-120.00   84
 38  \w      4.00 100.00   1.00   10.00    --   30.16  57.00 -90.00   96
 39  \w     37.00 116.00   1.00   10.00    --   30.16-178.00  90.00   79
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset/far, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0039939000
_diffrn_orient_matrix_UB_12      0.0384362000
_diffrn_orient_matrix_UB_13      0.0479617000
_diffrn_orient_matrix_UB_21      0.0067351000
_diffrn_orient_matrix_UB_22      0.0480446000
_diffrn_orient_matrix_UB_23      -0.0228867000
_diffrn_orient_matrix_UB_31      -0.0719437000
_diffrn_orient_matrix_UB_32      -0.0153682000
_diffrn_orient_matrix_UB_33      -0.0122609000
_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  0.0310
_diffrn_reflns_av_unetI/netI     0.0165
_diffrn_reflns_Laue_measured_fraction_full 0.9978
_diffrn_reflns_Laue_measured_fraction_max 0.9687
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            157579
_diffrn_reflns_point_group_measured_fraction_full 0.9978
_diffrn_reflns_point_group_measured_fraction_max 0.9687
_diffrn_reflns_theta_full        25.2417
_diffrn_reflns_theta_max         37.79
_diffrn_reflns_theta_min         3.20
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.819
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.480
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.88a (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    1.638
_exptl_crystal_description       needle
_exptl_crystal_F_000             775.164
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.13
_refine_diff_density_max         1.3314
_refine_diff_density_min         -1.3920
_refine_diff_density_rms         0.1062
_refine_ls_d_res_high            0.5799
_refine_ls_d_res_low             6.3634
_refine_ls_goodness_of_fit_ref   1.0511
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    39
_refine_ls_number_parameters     460
_refine_ls_number_reflns         16604
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0511
_refine_ls_R_factor_all          0.0228
_refine_ls_R_factor_gt           0.0180
_refine_ls_shift/su_max          -0.0004
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0106P)^2^+0.8563P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0365
_refine_ls_wR_factor_ref         0.0385
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              17
_reflns_limit_h_min              -18
_reflns_limit_k_max              20
_reflns_limit_k_min              -20
_reflns_limit_l_max              23
_reflns_limit_l_min              0
_reflns_number_gt                14979
_reflns_number_total             16604
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d4sc06782g2.cif
_cod_data_source_block           6
_cod_depositor_comments
'Adding full bibliography for 1573160--1573166.cif.'
_cod_database_code               1573165
_chemical_oxdiff_formula         C29H36GaI2N6
_chemical_oxdiff_usercomment     'Mounted by Arne'
_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
;
_olex2_refine_details
;
Refinement using NoSpherA2, an implementation of
NOn-SPHERical Atom-form-factors in Olex2.
Please cite:
F. Kleemiss et al. Chem. Sci. DOI 10.1039/D0SC05526C - 2021
NoSpherA2 implementation of HAR makes use of
tailor-made aspherical atomic form factors calculated
on-the-fly from a Hirshfeld-partitioned electron density (ED) - not from
spherical-atom form factors.

The ED is calculated from a gaussian basis set single determinant SCF
wavefunction - either Hartree-Fock or DFT using selected funtionals
 - for a fragment of the crystal.
This fragment can be embedded in an electrostatic crystal field by employing cluster charges
or modelled using implicit solvation models, depending on the software used.
The following options were used:
   SOFTWARE:       ORCA 5.0
   PARTITIONING:   NoSpherA2
   INT ACCURACY:   Normal
   METHOD:         PWLDA
   BASIS SET:      ECP-def2-QZVPP
   CHARGE:         0
   MULTIPLICITY:   1
   DATE:           2023-04-27_19-51-03
;
_olex2_date_sample_data_collection 2023-04-26
_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 1.252
_oxdiff_exptl_absorpt_empirical_full_min 0.858