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_1575306
_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_formula_moiety         'C42 H37 B F15 Ga N P, C3 H3'
_chemical_formula_sum            'C45 H40 B F15 Ga N P'
_chemical_formula_weight         991.28
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2022-08-24
_audit_creation_method
;
Olex2 1.5-beta
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_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            8
_cell_length_a                   15.4213(2)
_cell_length_b                   17.2470(3)
_cell_length_c                   31.7812(5)
_cell_measurement_reflns_used    37362
_cell_measurement_temperature    120.01(10)
_cell_measurement_theta_max      29.1490
_cell_measurement_theta_min      3.6000
_cell_volume                     8452.9(2)
_computing_cell_refinement       'CrysAlisPro 1.171.41.99a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.99a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.99a (Rigaku OD, 2021)'
_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_environment      N~2~
_diffrn_ambient_temperature      120.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.1574
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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    -83.00  13.00   1.00   15.00    --  -12.93 -53.00   8.00   96
  2  \w    -39.00  57.00   1.00   15.00    --  -12.93  53.00 153.00   96
  3  \w    -42.00  18.00   1.00   15.00    --  -12.93 -77.00 -60.00   60
  4  \w    -35.00  60.00   1.00   15.00    --  -12.93  38.00  60.00   95
  5  \w    -15.00  55.00   1.00   15.00    --   14.65 -99.00-180.00   70
  6  \w     39.00 101.00   1.00   15.00    --   14.65 178.00 -30.00   62
  7  \w    -86.00 -19.00   1.00   15.00    --  -12.93 -38.00  90.00   67
;
_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      -0.0068239000
_diffrn_orient_matrix_UB_12      -0.0041482000
_diffrn_orient_matrix_UB_13      -0.0219580000
_diffrn_orient_matrix_UB_21      -0.0345209000
_diffrn_orient_matrix_UB_22      -0.0261688000
_diffrn_orient_matrix_UB_23      0.0039712000
_diffrn_orient_matrix_UB_31      -0.0296229000
_diffrn_orient_matrix_UB_32      0.0314492000
_diffrn_orient_matrix_UB_33      0.0004279000
_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  0.0717
_diffrn_reflns_av_unetI/netI     0.0327
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       41
_diffrn_reflns_limit_l_min       -41
_diffrn_reflns_number            119571
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.484
_diffrn_reflns_theta_min         3.320
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.790
_exptl_absorpt_correction_T_max  0.89690
_exptl_absorpt_correction_T_min  0.89690
_exptl_absorpt_correction_type   sphere
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.99a (Rigaku Oxford Diffraction, 2021)
Spherical absorption correction
using equivalent radius and absorption coefficient.
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    1.558
_exptl_crystal_description       block
_exptl_crystal_F_000             4024
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.07
_exptl_crystal_size_rad          0.092
_refine_diff_density_max         0.545
_refine_diff_density_min         -0.359
_refine_diff_density_rms         0.064
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.074
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     614
_refine_ls_number_reflns         9662
_refine_ls_number_restraints     66
_refine_ls_restrained_S_all      1.079
_refine_ls_R_factor_all          0.0526
_refine_ls_R_factor_gt           0.0396
_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^)+(0.0333P)^2^+9.1347P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0877
_refine_ls_wR_factor_ref         0.0936
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7971
_reflns_number_total             9662
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4sc06894g3.cif
_cod_data_source_block           mc21058_refinalized
_cod_database_code               1575306
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C42 H37 B F15 Ga N P'
_chemical_oxdiff_usercomment     '@ 120 K RJS142'
_shelx_estimated_absorpt_t_max   0.947
_shelx_estimated_absorpt_t_min   0.786
_olex2_refinement_description
;
1. 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
2. Restrained distances
 C4A-C3A \\sim C4-C3
 with sigma of 0.02
 C3A-C5 \\sim C34-C33 \\sim C3-C2
 with sigma of 0.02
 C4A-C2 \\sim C5-C4
 with sigma of 0.02
 C6A-C5 \\sim C6-C2
 with sigma of 0.02
 C6A-C2 \\sim C6-C5
 with sigma of 0.02
 C5-C4A \\sim C5-C3
 with sigma of 0.02
 C2-C3A \\sim C2-C4
 with sigma of 0.02
3. Rigid body (RIGU) restrains
 C3A, C4A, C6A, C5, C2, C1, C7
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
4. Others
 Sof(H2B)=Sof(H5B)=Sof(C3A)=Sof(H3AA)=Sof(H3AB)=Sof(C4A)=Sof(H4AA)=Sof(H4AB)=
 Sof(C6A)=Sof(H6AA)=Sof(H6AB)=1-FVAR(1)
 Sof(H2A)=Sof(C3)=Sof(H3A)=Sof(H3B)=Sof(C4)=Sof(H4A)=Sof(H4B)=Sof(H5A)=Sof(C6)=
 Sof(H6A)=Sof(H6B)=FVAR(1)
5.a Ternary CH refined with riding coordinates:
 C2(H2A), C2(H2B), C5(H5A), C5(H5B)
5.b Secondary CH2 refined with riding coordinates:
 C3(H3A,H3B), C4(H4A,H4B), C6(H6A,H6B), C3A(H3AA,H3AB), C4A(H4AA,H4AB),
 C6A(H6AA,H6AB)
5.c Aromatic/amide H refined with riding coordinates:
 C18(H18), C20(H20), C43(H43), C44(H44), C45(H45)
5.d Idealised Me refined as rotating group:
 C9(H9A,H9B,H9C), C10(H10A,H10B,H10C), C11(H11A,H11B,H11C), C13(H13A,H13B,
 H13C), C14(H14A,H14B,H14C), C15(H15A,H15B,H15C), C22(H22A,H22B,H22C), C23(H23A,
 H23B,H23C), C24(H24A,H24B,H24C)
;
_shelx_res_checksum              36007
_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 1.234
_oxdiff_exptl_absorpt_empirical_full_min 0.833