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_1575298
_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         'C48 H74 Ga2 N2 P2, C6 D6'
_chemical_formula_sum            'C54 H74 D6 Ga2 N2 P2'
_chemical_formula_weight         964.61
_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
_atom_sites_solution_primary     dual
_audit_creation_date             2021-10-08
_audit_creation_method
;
Olex2 1.5-beta
(compiled 2021.08.20 svn.r13c46975 for OlexSys, GUI svn.r6405)
;
_audit_update_record
;
2024-09-16 deposited with the CCDC.	2025-04-10 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 93.272(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   13.2842(7)
_cell_length_b                   14.0429(7)
_cell_length_c                   13.7970(7)
_cell_measurement_reflns_used    9973
_cell_measurement_temperature    100.00
_cell_measurement_theta_max      26.37
_cell_measurement_theta_min      2.53
_cell_volume                     2569.6(2)
_computing_cell_refinement       'SAINT V8.40A (Bruker, 2019)'
_computing_data_collection       APEX4
_computing_data_reduction        'SAINT V8.40A (Bruker, 2019)'
_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  (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.00
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0550
_diffrn_reflns_av_unetI/netI     0.0259
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            119020
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.461
_diffrn_reflns_theta_min         2.192
_diffrn_source                   ImuS-Mo
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.146
_exptl_absorpt_correction_T_max  0.745372
_exptl_absorpt_correction_T_min  0.686413
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 TWINABS-2012/1 (Bruker,2012) was used for absorption correction.
 
For component 1:
 wR2(int) was 0.0678 before and 0.0448 after correction.
 
For component 2:
 wR2(int) was 0.1015 before and 0.0457 after correction.
 The Ratio of minimum to maximum transmission is 0.92.

Final HKLF 4 output contains 119020 reflections, Rint = 0.0550
 (56830 with I > 3sig(I), Rint = 0.0399)
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.247
_exptl_crystal_description       block
_exptl_crystal_F_000             1020
_exptl_crystal_recrystallization_method
'The material was recrystallised from d6-benzene by slow evaporation'
_exptl_crystal_size_max          0.155
_exptl_crystal_size_mid          0.091
_exptl_crystal_size_min          0.076
_refine_diff_density_max         0.339
_refine_diff_density_min         -0.388
_refine_diff_density_rms         0.066
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.171
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     424
_refine_ls_number_reflns         8531
_refine_ls_number_restraints     98
_refine_ls_restrained_S_all      1.171
_refine_ls_R_factor_all          0.0630
_refine_ls_R_factor_gt           0.0528
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+4.9662P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1116
_refine_ls_wR_factor_ref         0.1164
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7584
_reflns_number_total             8531
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4sc06894g3.cif
_cod_data_source_block           mc21046
_cod_database_code               1575298
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.918
_shelx_estimated_absorpt_t_min   0.842
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.5662(11)
 0.4338(11)
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
 P1-Ga1 \\sim P1-Ga1A
 with sigma of 0.02
 N1-Ga1 \\sim N1-Ga1A
 with sigma of 0.02
4. Rigid bond restraints
 C8A, C11A, C9A, C10A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
5. Uiso/Uaniso restraints and constraints
C8A \\sim C11A \\sim C9A \\sim C10A: within 2A with sigma of 0.04 and sigma for
terminal atoms of 0.08 within 2A
6. Rigid body (RIGU) restrains
 C8A, C11A, C9A, C10A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C8, C9, C11, C10
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C12, C13, C14, C15
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
7. Same fragment restrains
{C2, C3, C4, C5, C6} sigma for 1-2: 0.02, 1-3: 0.02
as in
{C2A, C3A, C4A, C5A, C6A}
{C8, C9, C10A, C11} sigma for 1-2: 0.02, 1-3: 0.02
as in
{C8A, C9A, C10, C11A}
{C12, C13, C14, C15} sigma for 1-2: 0.02, 1-3: 0.02
as in
{C12A, C13A, C14A, C15A}
8. Others
 Sof(Ga1A)=Sof(P1A)=Sof(C10A)=Sof(H10A)=Sof(H10B)=Sof(H10C)=Sof(C8A)=Sof(C9A)=
 Sof(H9AA)=Sof(H9AB)=Sof(H9AC)=Sof(C11A)=Sof(H11D)=Sof(H11E)=Sof(H11F)=
 Sof(C12A)=Sof(C13A)=Sof(H13D)=Sof(H13E)=Sof(H13F)=Sof(C14A)=Sof(H14D)=
 Sof(H14E)=Sof(H14F)=Sof(C15A)=Sof(H15D)=Sof(H15E)=Sof(H15F)=1-FVAR(1)
 Sof(Ga1)=Sof(P1)=Sof(C8)=Sof(C9)=Sof(H9A)=Sof(H9B)=Sof(H9C)=Sof(C11)=
 Sof(H11A)=Sof(H11B)=Sof(H11C)=Sof(C10)=Sof(H10D)=Sof(H10E)=Sof(H10F)=Sof(C12)=
 Sof(C13)=Sof(H13A)=Sof(H13B)=Sof(H13C)=Sof(C14)=Sof(H14A)=Sof(H14B)=Sof(H14C)=
 Sof(C15)=Sof(H15A)=Sof(H15B)=Sof(H15C)=FVAR(1)
 Sof(C2A)=Sof(H2A)=Sof(C3A)=Sof(H3AA)=Sof(H3AB)=Sof(C4A)=Sof(H4AA)=Sof(H4AB)=
 Sof(C5A)=Sof(H5A)=Sof(C6A)=Sof(H6AA)=Sof(H6AB)=1-FVAR(2)
 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)=FVAR(2)
9.a Ternary CH refined with riding coordinates:
 C2(H2), C5(H5), C2A(H2A), C5A(H5A)
9.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)
9.c Aromatic/amide H refined with riding coordinates:
 C18(H18), C20(H20), C25(D25), C26(D26), C27(D27)
9.d Idealised Me refined as rotating group:
 C9(H9A,H9B,H9C), C10A(H10A,H10B,H10C), C11(H11A,H11B,H11C), C9A(H9AA,H9AB,
 H9AC), C10(H10D,H10E,H10F), C11A(H11D,H11E,H11F), C13(H13A,H13B,H13C),
 C14(H14A,H14B,H14C), C15(H15A,H15B,H15C), C13A(H13D,H13E,H13F), C14A(H14D,H14E,
 H14F), C15A(H15D,H15E,H15F), C22(H22A,H22B,H22C), C23(H23A,H23B,H23C),
 C24(H24A,H24B,H24C)
;
_shelx_res_checksum              827
_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems Cryostream 800'
_olex2_exptl_crystal_mounting_method
'The crystal was mounted on a MITIGEN holder in Paratone oil'
_olex2_submission_original_sample_id RJS63
_olex2_submission_special_instructions 'No special instructions were received'