Reversible addition of ethene to gallium(i) monomers and dimers.
Schwamm, Ryan J.; Bhide, Malavika A.; Nichol, Gary S.; Cowley, Michael J.; Chemical science 16 (2025) 13333–13344; doi:10.1039/d4sc06894g

data_1575300
_publ_section_title
;
 Reversible addition of ethene to gallium(i) monomers and dimers.
;
_journal_issue                   29
_journal_name_full               'Chemical science'
_journal_page_first              13333
_journal_page_last               13344
_journal_paper_doi               10.1039/d4sc06894g
_journal_volume                  16
_journal_year                    2025
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C70 H86 Ga2 N2 P2'
_chemical_formula_sum            'C70 H86 Ga2 N2 P2'
_chemical_formula_weight         1156.78
_space_group_crystal_system      orthorhombic
_space_group_IT_number           29
_space_group_name_Hall           'P 2c -2ac'
_space_group_name_H-M_alt        'P c a 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2024-08-09
_audit_creation_method
;
Olex2 1.5-beta
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2024-09-16 deposited with the CCDC.	2025-04-10 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.02530(10)
_cell_length_b                   16.50370(10)
_cell_length_c                   26.14870(10)
_cell_measurement_reflns_used    60361
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      75.8510
_cell_measurement_theta_min      4.1190
_cell_volume                     6052.62(6)
_computing_cell_refinement       'CrysAlisPro 1.171.41.123a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.41.123a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.41.123a (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 1.5-beta (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-beta (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100.15
_diffrn_detector_area_resol_mean 5.1574
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 1.000
_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   -112.00 -64.00   1.00    2.50    --  -41.67-146.00  12.00   48
  2  \w    -87.00  -6.00   1.00    2.50    --  -41.67 125.00-103.00   81
  3  \w   -102.00 -16.00   1.00    2.50    --  -41.67 146.00  63.00   86
  4  \w     27.00  97.00   1.00    2.50    --   41.67-125.00 178.00   70
  5  \w     37.00 110.00   1.00    2.50    --   41.67-146.00  12.00   73
  6  \w     85.00 169.00   1.00   10.00    --  111.00 146.00  63.00   84
  7  \w     39.00 112.00   1.00   10.00    --  111.00-125.00 178.00   73
  8  \w     97.00 178.00   1.00   10.00    --  111.00 125.00-103.00   81
  9  \w     83.00 115.00   1.00   10.00    --  111.00-146.00  12.00   32
 10  \w    -63.00  29.00   1.00    2.50    --  -41.67  38.00  30.00   92
 11  \w   -114.00 -19.00   1.00    2.50    --  -41.67 -38.00  60.00   95
 12  \w   -127.00 -39.00   1.00    2.50    --  -41.67-178.00  90.00   88
 13  \w    -24.00  31.00   1.00    2.50    --  -41.67  38.00  60.00   55
 14  \w     10.00  41.00   1.00    2.50    --   41.67  80.00  62.58   31
 15  \w     10.00  42.00   1.00    2.50    --   41.67  82.00-103.08   32
 16  \w     39.00  89.00   1.00   10.00    --  111.00 -77.00 150.00   50
 17  \w    131.00 158.00   1.00   10.00    --  111.00  30.00  90.00   27
 18  \w     59.00  84.00   1.00   10.00    --  111.00 -61.00 -30.00   25
 19  \w     32.00  59.00   1.00   10.00    --  111.00 -94.00 -60.00   27
 20  \w     62.00 107.00   1.00   10.00    --  111.00 -94.00 -60.00   45
 21  \w     70.00  97.00   1.00   10.00    --  111.00-125.00 150.00   27
 22  \w    104.00 129.00   1.00   10.00    --  111.00 -77.00 120.00   25
 23  \w     59.00 112.00   1.00   10.00    --  111.00-125.00 -60.00   53
 24  \w     47.00 104.00   1.00   10.00    --  111.00-125.00-120.00   57
 25  \w     88.00 126.00   1.00   10.00    --  111.00  30.00  90.00   38
 26  \w     87.00 178.00   1.00   10.00    --  111.00  30.00  30.00   91
 27  \w     85.00 133.00   1.00   10.00    --  111.00 -61.00  30.00   48
 28  \w     88.00 150.00   1.00   10.00    --  111.00  30.00-120.00   62
 29  \w     31.00  61.00   1.00   10.00    --  111.00 -94.00-120.00   30
 30  \w     46.00  78.00   1.00   10.00    --  111.00 -45.00 120.00   32
 31  \w     93.00 132.00   1.00   10.00    --  111.00 -45.00 120.00   39
 32  \w     61.00  99.00   1.00   10.00    --  111.00-125.00 120.00   38
 33  \w    107.00 142.00   1.00   10.00    --  111.00 125.00  90.00   35
 34  \w    109.00 160.00   1.00   10.00    --  111.00 125.00  60.00   51
 35  \w     51.00  85.00   1.00   10.00    --  111.00 -77.00 120.00   34
 36  \w     84.00 111.00   1.00   10.00    --  111.00-125.00 -30.00   27
 37  \w    110.00 152.00   1.00   10.00    --  111.00 125.00 150.00   42
 38  \w    153.00 178.00   1.00   10.00    --  111.00 125.00 -60.00   25
 39  \w     41.00  66.00   1.00   10.00    --  111.00-105.00-167.01   25
 40  \w     33.00 147.00   1.00   10.00    --  111.00 -19.00  -4.61  114
 41  \w     43.00  73.00   1.00   10.00    --  111.00 -61.00  30.00   30
 42  \w    104.00 131.00   1.00   10.00    --  111.00 -85.00 -83.99   27
 43  \w     85.00 112.00   1.00   10.00    --  111.00-125.00  30.00   27
 44  \w     34.00  68.00   1.00   10.00    --  111.00 -85.00 -83.99   34
 45  \w     87.00 152.00   1.00   10.00    --  111.00  66.00-108.84   65
 46  \w     82.00 136.00   1.00   10.00    --  111.00 -61.00 120.00   54
 47  \w     92.00 123.00   1.00   10.00    --  111.00-138.00 175.23   31
 48  \w     83.00 108.00   1.00   10.00    --  111.00-105.00-167.01   25
 49  \w     62.00 112.00   1.00   10.00    --  111.00-125.00   0.00   50
 50  \w     53.00  80.00   1.00   10.00    --  111.00-125.00  30.00   27
 51  \w     82.00 107.00   1.00   10.00    --  111.00 -94.00-120.00   25
 52  \w     31.00 102.00   1.00   10.00    --  111.00 -94.00   0.00   71
 53  \w     84.00 134.00   1.00   10.00    --  111.00  61.00 -60.00   50
 54  \w     53.00 113.00   1.00   10.00    --  111.00 -30.00  30.00   60
 55  \w     98.00 133.00   1.00   10.00    --  111.00 125.00  30.00   35
 56  \w    153.00 178.00   1.00   10.00    --  111.00 125.00  30.00   25
 57  \w     94.00 131.00   1.00   10.00    --  111.00  30.00 120.00   37
 58  \w     41.00 107.00   1.00   10.00    --  111.00 -94.00  30.00   66
 59  \w     41.00  66.00   1.00   10.00    --  111.00 -94.00 150.00   25
 60  \w     72.00 101.00   1.00   10.00    --  111.00 -94.00 150.00   29
 61  \w    104.00 134.00   1.00   10.00    --  111.00 125.00-120.00   30
 62  \w    103.00 128.00   1.00   10.00    --  111.00 -77.00 150.00   25
 63  \w    141.00 168.00   1.00   10.00    --  111.00  41.00   7.18   27
 64  \w     89.00 138.00   1.00   10.00    --  111.00 -61.00 -30.00   49
 65  \w     83.00 112.00   1.00   10.00    --  111.00-125.00  60.00   29
 66  \w    103.00 146.00   1.00   10.00    --  111.00  77.00-150.00   43
 67  \w     80.00 107.00   1.00   10.00    --  111.00 -94.00  60.00   27
 68  \w     80.00 134.00   1.00   10.00    --  111.00 -30.00 120.00   54
 69  \w     93.00 118.00   1.00   10.00    --  111.00  30.00 150.00   25
 70  \w    110.00 135.00   1.00   10.00    --  111.00 -45.00-180.00   25
 71  \w    103.00 130.00   1.00   10.00    --  111.00 -61.00-120.00   27
 72  \w     42.00  81.00   1.00   10.00    --  111.00 -61.00  90.00   39
 73  \w     75.00 102.00   1.00   10.00    --  111.00 -67.00 177.43   27
 74  \w     88.00 115.00   1.00   10.00    --  111.00 -77.00-120.00   27
 75  \w     45.00  72.00   1.00   10.00    --  111.00 -30.00 120.00   27
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Rigaku Oxford Diffraction SuperNova'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0791
_diffrn_reflns_av_unetI/netI     0.0427
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            126586
_diffrn_reflns_point_group_measured_fraction_full 0.892
_diffrn_reflns_point_group_measured_fraction_max 0.878
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.012
_diffrn_reflns_theta_min         3.380
_exptl_absorpt_coefficient_mu    1.906
_exptl_absorpt_correction_T_max  0.87460
_exptl_absorpt_correction_T_min  0.87460
_exptl_absorpt_correction_type   sphere
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.123a (Rigaku Oxford Diffraction, 2022)
Spherical absorption correction
using equivalent radius and absorption coefficient.
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.269
_exptl_crystal_description       rod
_exptl_crystal_F_000             2448
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.04
_exptl_crystal_size_rad          0.047
_refine_diff_density_max         4.018
_refine_diff_density_min         -0.845
_refine_diff_density_rms         0.123
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.50(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     704
_refine_ls_number_reflns         11105
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0697
_refine_ls_R_factor_gt           0.0665
_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^)+(0.1409P)^2^+0.8918P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1649
_refine_ls_wR_factor_ref         0.1695
_reflns_Friedel_coverage         0.718
_reflns_Friedel_fraction_full    0.779
_reflns_Friedel_fraction_max     0.752
_reflns_number_gt                10449
_reflns_number_total             11105
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4sc06894g3.cif
_cod_data_source_block           mc22017_refinalized
_cod_database_code               1575300
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.928
_shelx_estimated_absorpt_t_min   0.599
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.50(3)
 0.50(3)
2. 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
3.a Ternary CH refined with riding coordinates:
 C2(H2), C5(H5), C36(H36), C39(H39)
3.b Secondary CH2 refined with riding coordinates:
 C3(H3A,H3B), C4(H4A,H4B), C6(H6A,H6B), C37(H37A,H37B), C38(H38A,H38B),
 C40(H40A,H40B), C69(H69A,H69B), C70(H70A,H70B)
3.c Aromatic/amide H refined with riding coordinates:
 C10(H10), C12(H12), C19(H19), C21(H21), C28(H28), C30(H30), C44(H44),
 C46(H46), C53(H53), C55(H55), C62(H62), C64(H64)
3.d Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C), C15(H15A,H15B,H15C), C16(H16A,H16B,H16C), C23(H23A,H23B,
 H23C), C24(H24A,H24B,H24C), C25(H25A,H25B,H25C), C32(H32A,H32B,H32C), C33(H33A,
 H33B,H33C), C34(H34A,H34B,H34C), C48(H48A,H48B,H48C), C49(H49A,H49B,H49C),
 C50(H50A,H50B,H50C), C57(H57A,H57B,H57C), C58(H58A,H58B,H58C), C59(H59A,H59B,
 H59C), C66(H66A,H66B,H66C), C67(H67A,H67B,H67C), C68(H68A,H68B,H68C)
;
_shelx_res_checksum              64182
_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems Cryostream 700+'
_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
;