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_1575305
_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         'C50 H78 Ga2 N2 P2, C6 D6'
_chemical_formula_sum            'C56 H78 D6 Ga2 N2 P2'
_chemical_formula_weight         992.66
_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_Hall           'P 2c -2n'
_space_group_name_H-M_alt        'P n a 21'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2022-08-26
_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            4
_cell_length_a                   28.6854(12)
_cell_length_b                   8.5990(3)
_cell_length_c                   21.4708(10)
_cell_measurement_reflns_used    7387
_cell_measurement_temperature    120.01(10)
_cell_measurement_theta_max      28.9400
_cell_measurement_theta_min      3.7680
_cell_volume                     5296.1(4)
_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(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0521
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.877
_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  12.00   1.00   30.00    --  -19.31 109.00 -29.00   77
  2  \w    -15.00  89.00   1.00   30.00    --   21.19  19.00-142.00  104
  3  \w      6.00  38.00   1.00   30.00    --   21.19  77.00-180.00   32
  4  \w     -7.00  25.00   1.00   30.00    --   21.19  77.00 150.00   32
;
_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      -0.0053373000
_diffrn_orient_matrix_UB_12      0.0144357000
_diffrn_orient_matrix_UB_13      0.0317446000
_diffrn_orient_matrix_UB_21      0.0235128000
_diffrn_orient_matrix_UB_22      -0.0152146000
_diffrn_orient_matrix_UB_23      0.0081724000
_diffrn_orient_matrix_UB_31      0.0054443000
_diffrn_orient_matrix_UB_32      0.0797812000
_diffrn_orient_matrix_UB_33      -0.0041923000
_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  0.0577
_diffrn_reflns_av_unetI/netI     0.0642
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.877
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -39
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            29105
_diffrn_reflns_point_group_measured_fraction_full 0.644
_diffrn_reflns_point_group_measured_fraction_max 0.546
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.568
_diffrn_reflns_theta_min         3.325
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.114
_exptl_absorpt_correction_T_max  0.388
_exptl_absorpt_correction_T_min  0.204
_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            colourless
_exptl_crystal_density_diffrn    1.245
_exptl_crystal_description       block
_exptl_crystal_F_000             2104
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.579
_refine_diff_density_min         -0.576
_refine_diff_density_rms         0.086
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.490(12)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.081
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     652
_refine_ls_number_reflns         8872
_refine_ls_number_restraints     100
_refine_ls_restrained_S_all      1.078
_refine_ls_R_factor_all          0.0588
_refine_ls_R_factor_gt           0.0446
_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^)+(0.0273P)^2^+0.6456P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0763
_refine_ls_wR_factor_ref         0.0828
_reflns_Friedel_coverage         0.216
_reflns_Friedel_fraction_full    0.270
_reflns_Friedel_fraction_max     0.199
_reflns_number_gt                7592
_reflns_number_total             8872
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4sc06894g3.cif
_cod_data_source_block           rjs311
_cod_database_code               1575305
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C H N P Ga'
_chemical_oxdiff_usercomment     '@ 120 K, Ga(I) + ethene'
_shelx_estimated_absorpt_t_max   0.842
_shelx_estimated_absorpt_t_min   0.724
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.510(12)
 0.490(12)
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. Restrained distances
 C6A-C2A \\sim C6-C2
 with sigma of 0.02
 C6A-C5A \\sim C6-C5
 with sigma of 0.02
 C7-C2A \\sim C2-C1
 with sigma of 0.02
 C3A-C2A \\sim C3-C2
 with sigma of 0.02
 C5A-C1 \\sim C7-C5
 with sigma of 0.02
 C4A-C3A \\sim C4-C3
 with sigma of 0.02
 C5A-C4A \\sim C5-C4
 with sigma of 0.02
 C28A-C27A \\sim C28-C27
 with sigma of 0.02
 C30A-C26 \\sim C30-C29
 with sigma of 0.02
 C28A-C26 \\sim C29-C28
 with sigma of 0.02
 C29-C27A \\sim C27-C26
 with sigma of 0.02
 C30A-C29 \\sim C30-C26
 with sigma of 0.02
4. Rigid body (RIGU) restrains
 C3A, C5A, C2A, C4A, C6A, C1, C7
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C27A, C30A, C28A, C26, C29
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
5. Others
 Sof(C3A)=Sof(H3AA)=Sof(H3AB)=Sof(C4A)=Sof(H4AA)=Sof(H4AB)=Sof(C6A)=Sof(H6AA)=
 Sof(H6AB)=Sof(C2A)=Sof(H2A)=Sof(C5A)=Sof(H5A)=1-FVAR(1)
 Sof(C4)=Sof(H4A)=Sof(H4B)=Sof(C3)=Sof(H3A)=Sof(H3B)=Sof(C2)=Sof(H2)=Sof(C5)=
 Sof(H5)=Sof(C6)=Sof(H6A)=Sof(H6B)=FVAR(1)
 Sof(H26A)=Sof(H29A)=Sof(C27A)=Sof(H27C)=Sof(H27D)=Sof(C28A)=Sof(H28C)=
 Sof(H28D)=Sof(C30A)=Sof(H30C)=Sof(H30D)=1-FVAR(2)
 Sof(H26)=Sof(H29)=Sof(C30)=Sof(H30A)=Sof(H30B)=Sof(C27)=Sof(H27A)=Sof(H27B)=
 Sof(C28)=Sof(H28A)=Sof(H28B)=FVAR(2)
6.a Ternary CH refined with riding coordinates:
 C26(H26), C26(H26A), C29(H29), C29(H29A), C2(H2), C5(H5), C2A(H2A), C5A(H5A)
6.b Secondary CH2 refined with riding coordinates:
 C49(H49A,H49B), C50(H50A,H50B), C4(H4A,H4B), C3(H3A,H3B), C6(H6A,H6B),
 C30(H30A,H30B), C27(H27A,H27B), C28(H28A,H28B), C3A(H3AA,H3AB), C4A(H4AA,H4AB),
  C6A(H6AA,H6AB), C27A(H27C,H27D), C28A(H28C,H28D), C30A(H30C,H30D)
6.c Aromatic/amide H refined with riding coordinates:
 C20(H20), C18(H18), C44(H44), C42(H42), C51(D51), C53(D53), C52(D52),
 C56(D56), C54(D54), C55(D55)
6.d Idealised Me refined as rotating group:
 C39(H39A,H39B,H39C), C22(H22A,H22B,H22C), C33(H33A,H33B,H33C), C15(H15A,H15B,
 H15C), C35(H35A,H35B,H35C), C24(H24A,H24B,H24C), C38(H38A,H38B,H38C), C14(H14A,
 H14B,H14C), C46(H46A,H46B,H46C), C23(H23A,H23B,H23C), C34(H34A,H34B,H34C),
 C47(H47A,H47B,H47C), C9(H9A,H9B,H9C), C13(H13A,H13B,H13C), C37(H37A,H37B,H37C),
  C48(H48A,H48B,H48C), C11(H11A,H11B,H11C), C10(H10A,H10B,H10C)
;
_shelx_res_checksum              47029
_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 1.144
_oxdiff_exptl_absorpt_empirical_full_min 0.746