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_1575301
_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         'C34 H41 Ga N P'
_chemical_formula_sum            'C34 H41 Ga N P'
_chemical_formula_weight         564.37
_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             2022-08-22
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2024-09-16 deposited with the CCDC.	2025-04-10 downloaded from the CCDC.
;
_cell_angle_alpha                80.922(3)
_cell_angle_beta                 76.755(3)
_cell_angle_gamma                75.256(3)
_cell_formula_units_Z            2
_cell_length_a                   9.8258(3)
_cell_length_b                   10.6897(4)
_cell_length_c                   15.1671(6)
_cell_measurement_reflns_used    12262
_cell_measurement_temperature    120.00(10)
_cell_measurement_theta_max      28.7570
_cell_measurement_theta_min      3.8500
_cell_volume                     1491.24(10)
_computing_cell_refinement       'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (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      120.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0521
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.892
_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    -65.00   8.00   1.00   15.00    --  -16.31 114.00 172.00   73
  2  \w     -8.00  67.00   1.00   15.00    --   18.03-114.00  81.00   75
  3  \w    -39.00  12.00   1.00   15.00    --  -16.31 -77.00 120.00   51
  4  \w    -35.00  52.00   1.00   15.00    --  -16.31  57.00  60.00   87
  5  \w    -85.00   2.00   1.00   15.00    --  -16.31 -57.00 150.00   87
  6  \w    -35.00  52.00   1.00   15.00    --  -16.31  57.00 -60.00   87
  7  \w    -20.00  59.00   1.00   15.00    --   18.03 -99.00   0.00   79
  8  \w    -11.00  39.00   1.00   15.00    --   18.03  77.00-180.00   50
  9  \w    -85.00 -14.00   1.00   15.00    --  -16.31 -57.00 -90.00   71
 10  \w    -39.00  12.00   1.00   15.00    --  -16.31 -77.00-150.00   51
 11  \w    -11.00  39.00   1.00   15.00    --   18.03  77.00  90.00   50
 12  \w     -4.00  89.00   1.00   15.00    --   18.03  38.00  90.00   93
 13  \w     39.00  92.00   1.00   15.00    --   18.03 178.00-120.00   53
 14  \w      0.00  86.00   1.00   15.00    --   18.03  57.00   0.00   86
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0027763000
_diffrn_orient_matrix_UB_12      0.0453315000
_diffrn_orient_matrix_UB_13      0.0286574000
_diffrn_orient_matrix_UB_21      0.0040503000
_diffrn_orient_matrix_UB_22      0.0480520000
_diffrn_orient_matrix_UB_23      -0.0379335000
_diffrn_orient_matrix_UB_31      -0.0759928000
_diffrn_orient_matrix_UB_32      0.0199237000
_diffrn_orient_matrix_UB_33      0.0086053000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0406
_diffrn_reflns_av_unetI/netI     0.0401
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.892
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            32783
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.892
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.303
_diffrn_reflns_theta_min         3.233
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.999
_exptl_absorpt_correction_T_max  0.460
_exptl_absorpt_correction_T_min  0.199
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.93a (Rigaku Oxford Diffraction, 2020)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear yellow'
_exptl_crystal_density_diffrn    1.257
_exptl_crystal_description       block
_exptl_crystal_F_000             596
_exptl_crystal_size_max          0.235
_exptl_crystal_size_mid          0.185
_exptl_crystal_size_min          0.115
_refine_diff_density_max         0.413
_refine_diff_density_min         -0.335
_refine_diff_density_rms         0.064
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.929
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     343
_refine_ls_number_reflns         7290
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.929
_refine_ls_R_factor_all          0.0492
_refine_ls_R_factor_gt           0.0391
_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^)+(0.1000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1193
_refine_ls_wR_factor_ref         0.1278
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6256
_reflns_number_total             7290
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4sc06894g3.cif
_cod_data_source_block           rjs351_pent_autored
_cod_database_code               1575301
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C H N P Ga'
_chemical_oxdiff_usercomment
'120K, 100 % scr, Tri P, LmesmesGa from pentane'
_shelx_estimated_absorpt_t_max   0.894
_shelx_estimated_absorpt_t_min   0.799
_reflns_odcompleteness_completeness 99.80
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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.a Ternary CH refined with riding coordinates:
 C2(H2), C5(H5)
2.b Secondary CH2 refined with riding coordinates:
 C3(H3A,H3B), C4(H4A,H4B), C6(H6A,H6B)
2.c Aromatic/amide H refined with riding coordinates:
 C10(H10), C12(H12), C19(H19), C21(H21), C28(H28), C30(H30)
2.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)
;
_shelx_res_checksum              2114
_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 1.284
_oxdiff_exptl_absorpt_empirical_full_min 0.684