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_1573162
_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
'C73.875 H78 Fe1.969 Ga2 I0.063 N4 O7.875, 1.5(C6 H6)'
_chemical_formula_sum            'C82.88 H87 Fe1.97 Ga2 I0.06 N4 O7.88'
_chemical_formula_weight         1522.77
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2023-12-15
_audit_creation_method
;
Olex2 1.5-ac6-012
(compiled 2023.08.24 svn.re1ec1418 for Rigaku Oxford Diffraction, GUI svn.r6817)
;
_audit_update_record
;
2024-02-23 deposited with the CCDC.	2024-11-14 downloaded from the CCDC.
;
_cell_angle_alpha                98.115(2)
_cell_angle_beta                 96.616(2)
_cell_angle_gamma                102.807(2)
_cell_formula_units_Z            2
_cell_length_a                   10.8571(2)
_cell_length_b                   14.3020(3)
_cell_length_c                   25.6182(5)
_cell_measurement_reflns_used    19734
_cell_measurement_temperature    100.0(1)
_cell_measurement_theta_max      76.2220
_cell_measurement_theta_min      3.3590
_cell_volume                     3795.66(14)
_computing_cell_refinement       'CrysAlisPro 1.171.43.95a (Rigaku OD, 2023)'
_computing_data_collection
'CrysAlisPro system (CCD 42.94a 64-bit (release 21-06-2023))'
_computing_data_reduction        'CrysAlisPro 1.171.43.95a (Rigaku OD, 2023)'
_computing_molecular_graphics    'Olex2 1.5-ac6-012 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-ac6-012 (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 1.000
_diffrn_measured_fraction_theta_max 0.979
_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    -92.00  44.00   1.00   10.00    --  -38.50   0.00-150.00  136
  2  \w    -48.00  -8.00   1.00   10.00    --  -38.50 125.00-180.00   40
  3  \w    -52.00  12.00   1.00   10.00    --  -38.50  38.00  90.00   64
  4  \w     31.00  90.00   1.00   10.00    --   42.70-125.00   0.00   59
  5  \w     30.00  89.00   1.00   10.00    --   42.70-125.00-180.00   59
  6  \w    135.00 177.00   1.00   30.00    --  111.00  15.00 -60.00   42
  7  \w     83.00 110.00   1.00   30.00    --  111.00  15.00 -60.00   27
  8  \w     47.00 109.00   1.00   30.00    --  111.00-108.00-172.93   62
  9  \w    122.00 178.00   1.00   30.00    --  111.00  71.00 -54.36   56
 10  \w     83.00 115.00   1.00   30.00    --  111.00  71.00 -54.36   32
 11  \w     45.00  72.00   1.00   30.00    --  111.00-106.00  87.00   27
 12  \w     86.00 113.00   1.00   30.00    --  111.00-125.00 -90.00   27
 13  \w     45.00 120.00   1.00   30.00    --  111.00 -30.00   0.00   75
 14  \w     58.00 105.00   1.00   30.00    --  111.00 -77.00-180.00   47
 15  \w     89.00 173.00   1.00   30.00    --  111.00  45.00   0.00   84
 16  \w     60.00 101.00   1.00   30.00    --  111.00 -94.00 -30.00   41
 17  \w     45.00  88.00   1.00   30.00    --  111.00-125.00-180.00   43
 18  \w    112.00 139.00   1.00   30.00    --  111.00 -77.00-180.00   27
 19  \w     45.00 124.00   1.00   30.00    --  111.00 -45.00 150.00   79
 20  \w     95.00 176.00   1.00   30.00    --  111.00  45.00  30.00   81
 21  \w    118.00 177.00   1.00   30.00    --  111.00  77.00  60.00   59
 22  \w     43.00 132.00   1.00   30.00    --  111.00 -61.00 -60.00   89
 23  \w     60.00 108.00   1.00   30.00    --  111.00-103.00 -66.88   48
 24  \w     80.00 107.00   1.00   30.00    --  111.00 -94.00   0.00   27
 25  \w     54.00 107.00   1.00   30.00    --  111.00 -94.00  30.00   53
 26  \w     53.00 108.00   1.00   30.00    --  111.00-103.00 118.64   55
;
_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      -0.1105995000
_diffrn_orient_matrix_UB_12      0.0000141000
_diffrn_orient_matrix_UB_13      -0.0434543000
_diffrn_orient_matrix_UB_21      -0.0542059000
_diffrn_orient_matrix_UB_22      0.0636400000
_diffrn_orient_matrix_UB_23      0.0407088000
_diffrn_orient_matrix_UB_31      0.0806409000
_diffrn_orient_matrix_UB_32      0.0923302000
_diffrn_orient_matrix_UB_33      -0.0152079000
_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  0.0297
_diffrn_reflns_av_unetI/netI     0.0346
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.979
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            34577
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.979
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.423
_diffrn_reflns_theta_min         3.392
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    4.430
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.398
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.43.95a (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 orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.332
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1584
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.866
_refine_diff_density_min         -0.728
_refine_diff_density_rms         0.067
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     927
_refine_ls_number_reflns         15591
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.021
_refine_ls_R_factor_all          0.0405
_refine_ls_R_factor_gt           0.0373
_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^)+(0.0656P)^2^+1.1645P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0994
_refine_ls_wR_factor_ref         0.1027
_reflns_Friedel_coverage         0.000
_reflns_number_gt                14480
_reflns_number_total             15591
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4sc06782g2.cif
_cod_data_source_block           9
_cod_depositor_comments
'Adding full bibliography for 1573160--1573166.cif.'
_cod_original_cell_volume        3795.66(13)
_cod_database_code               1573162
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C83H88Fe2Ga2N4O8
_chemical_oxdiff_usercomment     'Mounted by Arne'
_shelx_estimated_absorpt_t_max   0.666
_shelx_estimated_absorpt_t_min   0.298
_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. Others
 Sof(I1)=Sof(I2)=1-FVAR(1)
 Sof(Fe2)=Sof(O5)=Sof(O6)=Sof(O7)=Sof(O8)=Sof(C71)=Sof(C72)=Sof(C73)=Sof(C74)=
 FVAR(1)
3.a Ternary CH refined with riding coordinates:
 C19(H19), C22(H22), C31(H31), C34(H34), C49(H49), C52(H52), C61(H61), C64(H64)
3.b Aromatic/amide H refined with riding coordinates:
 C8(H8), C9(H9), C10(H10), C11(H11), C12(H12), C15(H15), C16(H16), C17(H17),
 C27(H27), C28(H28), C29(H29), C38(H38), C39(H39), C40(H40), C41(H41), C42(H42),
  C45(H45), C46(H46), C47(H47), C57(H57), C58(H58), C59(H59), C75(H75),
 C76(H76), C77(H77), C78(H78), C79(H79), C80(H80), C81(H81), C82(H82), C83(H83)
3.c Idealised Me refined as rotating group:
 C20(H20A,H20B,H20C), C21(H21A,H21B,H21C), C23(H23A,H23B,H23C), C24(H24A,H24B,
 H24C), C32(H32A,H32B,H32C), C33(H33A,H33B,H33C), C35(H35A,H35B,H35C), C36(H36A,
 H36B,H36C), C50(H50A,H50B,H50C), C51(H51A,H51B,H51C), C53(H53A,H53B,H53C),
 C54(H54A,H54B,H54C), C62(H62A,H62B,H62C), C63(H63A,H63B,H63C), C65(H65A,H65B,
 H65C), C66(H66A,H66B,H66C)
;
_shelx_res_checksum              96243
_shelx_hkl_checksum              77290
_olex2_date_sample_data_collection 2023-07-16
_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 1.894
_oxdiff_exptl_absorpt_empirical_full_min 0.758