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_1575303
_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         'C52 H41 B F15 Ga N P'
_chemical_formula_sum            'C52 H41 B F15 Ga N P'
_chemical_formula_weight         1076.36
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_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                 92.238(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.3929(5)
_cell_length_b                   14.7735(5)
_cell_length_c                   21.6915(6)
_cell_measurement_reflns_used    10378
_cell_measurement_temperature    120.01(11)
_cell_measurement_theta_max      28.0450
_cell_measurement_theta_min      3.7610
_cell_volume                     4608.8(3)
_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 1.5-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(11)
_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 0.858
_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  56.00   1.00   22.50    --  -16.31  20.00-175.00  109
  2  \w    -79.00 -34.00   1.00   22.50    --  -16.31 -20.00  16.00   45
  3  \w     65.00  90.00   1.00   22.50    --   18.03  20.00-175.00   25
  4  \w    -24.00   1.00   1.00   22.50    --   18.03 -20.00  16.00   25
  5  \w    -87.00 -40.00   1.00   22.50    --  -16.31-178.00-180.00   47
  6  \w    -67.00 -42.00   1.00   22.50    --  -16.31-178.00-120.00   25
  7  \w    -13.00  18.00   1.00   22.50    --  -16.31  77.00  30.00   31
  8  \w    -38.00  39.00   1.00   22.50    --  -16.31  77.00  60.00   77
  9  \w     -6.00  39.00   1.00   22.50    --   18.03  77.00-120.00   45
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Rigaku Oxford Diffraction XCalibur'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0264337000
_diffrn_orient_matrix_UB_12      0.0022439000
_diffrn_orient_matrix_UB_13      0.0268801000
_diffrn_orient_matrix_UB_21      0.0399063000
_diffrn_orient_matrix_UB_22      -0.0123711000
_diffrn_orient_matrix_UB_23      0.0183235000
_diffrn_orient_matrix_UB_31      0.0119107000
_diffrn_orient_matrix_UB_32      0.0463214000
_diffrn_orient_matrix_UB_33      0.0035911000
_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  0.0469
_diffrn_reflns_av_unetI/netI     0.0589
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.858
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            42048
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.858
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.270
_diffrn_reflns_theta_min         3.256
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.732
_exptl_absorpt_correction_T_max  0.502
_exptl_absorpt_correction_T_min  0.292
_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 colourless'
_exptl_crystal_density_diffrn    1.551
_exptl_crystal_description       block
_exptl_crystal_F_000             2184
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.713
_refine_diff_density_min         -0.584
_refine_diff_density_rms         0.071
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     698
_refine_ls_number_reflns         10782
_refine_ls_number_restraints     83
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0780
_refine_ls_R_factor_gt           0.0504
_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^)+(0.0266P)^2^+4.5933P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0882
_refine_ls_wR_factor_ref         0.0978
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8101
_reflns_number_total             10782
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4sc06894g3.cif
_cod_data_source_block           rjs355
_cod_database_code               1575303
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C H N P Ga B F'
_chemical_oxdiff_usercomment     'LmesmesGa-BCF, 120K, 100%, moderate'
_shelx_estimated_absorpt_t_max   0.911
_shelx_estimated_absorpt_t_min   0.821
_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
 C7-C5 \\sim C5A-C1
 with sigma of 0.02
 C4A-C3A \\sim C4-C3
 with sigma of 0.02
 C1A-C2A \\sim C2-C1
 with sigma of 0.02
 C3A-C2A \\sim C3-C2
 with sigma of 0.02
 C6A-C2A \\sim C6-C2
 with sigma of 0.02
 C5A-C4A \\sim C5-C4
 with sigma of 0.02
 C6A-C5A \\sim C6-C5
 with sigma of 0.02
3. Rigid bond restraints
 C1, C3A, C5A, C4A, C1A, C6A, C2A
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
4. Uiso/Uaniso restraints and constraints
Uanis(C1A) = Uanis(C7)
5. Rigid body (RIGU) restrains
 C1, C3A, C5A, C4A, C1A, C6A, C2A
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
6. Others
 Sof(C3A)=Sof(H3AA)=Sof(H3AB)=Sof(C1A)=Sof(C2A)=Sof(H2A)=Sof(C4A)=Sof(H4AA)=
 Sof(H4AB)=Sof(C5A)=Sof(H5A)=Sof(C6A)=Sof(H6AA)=Sof(H6AB)=1-FVAR(1)
 Sof(C2)=Sof(H2)=Sof(C3)=Sof(H3A)=Sof(H3B)=Sof(C4)=Sof(H4A)=Sof(H4B)=Sof(C5)=
 Sof(H5)=Sof(C6)=Sof(H6A)=Sof(H6B)=Sof(C7)=FVAR(1)
7.a Ternary CH refined with riding coordinates:
 C2(H2), C5(H5), C2A(H2A), C5A(H5A)
7.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)
7.c Aromatic/amide H refined with riding coordinates:
 C10(H10), C12(H12), C19(H19), C21(H21), C28(H28), C30(H30)
7.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              10772
_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 1.167
_oxdiff_exptl_absorpt_empirical_full_min 0.845