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_1575302
_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         'C24 H37 Ga N P, B C24 F20, 2(C6 H5 F)'
_chemical_formula_sum            'C60 H47 B F22 Ga N P'
_chemical_formula_weight         1311.48
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2025-03-10
_audit_creation_method
;
Olex2 1.5-beta
(compiled 2025.03.04 svn.red2d20d0 for OlexSys, GUI svn.r7188)
;
_audit_update_record
;
2025-03-21 deposited with the CCDC.	2025-04-10 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 116.108(9)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.0973(13)
_cell_length_b                   23.9872(10)
_cell_length_c                   17.0383(9)
_cell_measurement_reflns_used    6970
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      69.9460
_cell_measurement_theta_min      3.2640
_cell_volume                     5540.7(7)
_computing_cell_refinement       'CrysAlisPro 1.171.43.143a (Rigaku OD, 2024)'
_computing_data_collection
'CrysAlisPro system (CCD 43.143a 64-bit (release 25-10-2024))'
_computing_data_reduction        'CrysAlisPro 1.171.43.143a (Rigaku OD, 2024)'
_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      100.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            'HyPix-Arc 100'
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.932
_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    -45.00  -8.00   0.50    1.00    --   40.06 -19.00 150.00   74
  2  \w     13.00  42.00   0.50    1.00    --  -43.56  19.00 150.00   58
  3  \w     11.00  42.00   0.50    1.00    --  -43.56  19.00 120.00   62
  4  \w     11.00  42.00   0.50    1.00    --  -43.56  19.00  90.00   62
  5  \w    -99.00 -11.00   0.50    1.00    --  -43.56 125.00-180.00  176
  6  \w     12.00  42.00   0.50    1.00    --  -43.56  19.00  60.00   60
  7  \w   -163.00-105.00   0.50    4.00    --  -91.57 -77.00-150.00  116
  8  \w    -65.00 -21.00   0.50    4.00    --  -91.57  77.00 150.00   88
  9  \w   -157.00 -66.00   0.50    4.00    --  -91.57 -30.00-120.00  182
 10  \w     31.00  74.00   0.50    4.00    --  102.22 -77.00 -60.00   86
 11  \w     27.00  53.00   0.50    4.00    --  102.22 -61.00   0.00   52
 12  \w     25.00  92.00   0.50    4.00    --  102.22 -95.00 120.00  134
 13  \w     26.00  52.00   0.50    4.00    --  102.22 -61.00-120.00   52
 14  \w     45.00  74.00   0.50    4.00    --  110.03 -77.00 -30.00   58
 15  \w     34.00  60.00   0.50    4.00    --  110.03-125.00-150.00   52
 16  \w     89.00 172.00   0.50    4.00    --  110.03  30.00-120.00  166
 17  \w     50.00  91.00   0.50    4.00    --  110.03 -95.00 -90.00   82
 18  \w     74.00 101.00   0.50    4.00    --  110.03-125.00-150.00   54
 19  \w    -39.00 -11.00   0.50    1.00    --   40.44 -38.00 -90.00   56
 20  \w    -38.00 -12.00   0.50    1.00    --   40.44 -19.00-180.00   52
 21  \w     -6.00  20.00   0.50    1.00    --   40.44 -38.00 -90.00   52
 22  \w    -18.00  25.00   0.50    1.00    --  -43.56  38.00  30.00   86
 23  \w     -5.00  38.00   0.50    1.00    --  -43.56  38.00 -60.00   86
 24  \w    -14.00  12.00   0.50    1.00    --  -43.56  38.00 -90.00   52
 25  \w     13.00  39.00   0.50    1.00    --  -43.56  19.00 -90.00   52
 26  \w     11.00  36.00   0.50    1.00    --  -43.56  19.00 -30.00   50
 27  \w     12.00  38.00   0.50    1.00    --  -43.56  19.00-180.00   52
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, HyPix-Arc 100'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.1024570000
_diffrn_orient_matrix_UB_12      0.0120219000
_diffrn_orient_matrix_UB_13      0.0753185000
_diffrn_orient_matrix_UB_21      0.0492187000
_diffrn_orient_matrix_UB_22      -0.0249859000
_diffrn_orient_matrix_UB_23      -0.0543437000
_diffrn_orient_matrix_UB_31      -0.0001092000
_diffrn_orient_matrix_UB_32      0.0578819000
_diffrn_orient_matrix_UB_33      -0.0390155000
_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  0.0489
_diffrn_reflns_av_unetI/netI     0.0606
_diffrn_reflns_Laue_measured_fraction_full 0.980
_diffrn_reflns_Laue_measured_fraction_max 0.932
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            25453
_diffrn_reflns_point_group_measured_fraction_full 0.980
_diffrn_reflns_point_group_measured_fraction_max 0.932
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.533
_diffrn_reflns_theta_min         3.260
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'PhotonJet R (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.997
_exptl_absorpt_correction_T_max  0.91713
_exptl_absorpt_correction_T_min  0.91713
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.43.143a (Rigaku Oxford Diffraction, 2024)
Spherical absorption correction
using equivalent radius and absorption coefficient.
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'dark green'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.572
_exptl_crystal_description       block
_exptl_crystal_F_000             2652
_exptl_crystal_size_max          0.102
_exptl_crystal_size_mid          0.049
_exptl_crystal_size_min          0.024
_refine_diff_density_max         1.598
_refine_diff_density_min         -0.796
_refine_diff_density_rms         0.153
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.185
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     795
_refine_ls_number_reflns         10828
_refine_ls_number_restraints     45
_refine_ls_restrained_S_all      1.183
_refine_ls_R_factor_all          0.1397
_refine_ls_R_factor_gt           0.1136
_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^)+(0.1090P)^2^+28.6281P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2778
_refine_ls_wR_factor_ref         0.2932
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8253
_reflns_number_total             10828
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4sc06894g3.cif
_cod_data_source_block           mc24013_auto
_cod_database_code               1575302
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C120 H94 B2 F44 Ga2 N2 P2'
_chemical_oxdiff_usercomment     '@ 100 K MAB319'
_shelx_estimated_absorpt_t_max   0.954
_shelx_estimated_absorpt_t_min   0.822
_diffrn_oxdiff_digest_hkl
;
43959035d1e478051d5c179610f289b85879a8
;
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.9908(6)
 0.0092(6)
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. Rigid body (RIGU) restrains
 F86, C80, C85, C81, C83, C84, C82
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Sof(H73)=Sof(F5)=1-FVAR(1)
 Sof(H77)=Sof(F79)=FVAR(1)
5.a Ternary CH refined with riding coordinates:
 C5(H5), C2(H2)
5.b Secondary CH2 refined with riding coordinates:
 C4(H4A,H4B), C8(H8A,H8B), C3(H3A,H3B)
5.c Aromatic/amide H refined with riding coordinates:
 C14(H14), C12(H12), C74(H74), C75(H75), C78(H78), C76(H76), C73(H73),
 C77(H77), C85(H85), C81(H81), C83(H83), C84(H84), C82(H82)
5.d Idealised Me refined as rotating group:
 C17(H17A,H17B,H17C), C16(H16A,H16B,H16C), C21(H21A,H21B,H21C), C26(H26A,H26B,
 H26C), C24(H24A,H24B,H24C), C18(H18A,H18B,H18C), C27(H27A,H27B,H27C), C25(H25A,
 H25B,H25C), C23(H23A,H23B,H23C)
;
_shelx_res_checksum              11799
_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems Cryostream 1000'
_olex2_exptl_crystal_mounting_method
'The crystal was mounted on a MITIGEN holder in paratone oil'
_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 1.573
_oxdiff_exptl_absorpt_empirical_full_min 0.655