The structures and reactivity of NHC-supported copper(i) triphenylgermyls
Charman, Rex S. C.; Evans, Nick J.; English, Laura E.; Neale, Samuel E.; Vasko, Petra; Mahon, Mary F.; Liptrot, David J.; Chemical Science 15 (2024) 584–593; doi:10.1039/D3SC05862J

data_1570638
_publ_section_title
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 The structures and reactivity of NHC-supported copper(i) triphenylgermyls
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_journal_issue                   2
_journal_name_full               'Chemical Science'
_journal_page_first              584
_journal_page_last               593
_journal_paper_doi               10.1039/D3SC05862J
_journal_volume                  15
_journal_year                    2024
_chemical_formula_moiety         '2(C45 H51 Cu Ge N2)'
_chemical_formula_sum            'C90 H102 Cu2 Ge2 N4'
_chemical_formula_weight         1512.01
_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
_audit_creation_date             2023-11-28
_audit_creation_method
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_audit_update_record
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2023-11-28 deposited with the CCDC.	2023-12-01 downloaded from the CCDC.
;
_cell_angle_alpha                86.2830(10)
_cell_angle_beta                 77.2810(10)
_cell_angle_gamma                73.4720(10)
_cell_formula_units_Z            2
_cell_length_a                   11.02640(10)
_cell_length_b                   19.2655(3)
_cell_length_c                   20.3965(3)
_cell_measurement_reflns_used    30956
_cell_measurement_temperature    150.01(10)
_cell_measurement_theta_max      73.0520
_cell_measurement_theta_min      4.2810
_cell_volume                     4051.84(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 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      150.01(10)
_diffrn_detector_area_resol_mean 8.1150
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, EosS2'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0274
_diffrn_reflns_av_unetI/netI     0.0242
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            48122
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.348
_diffrn_reflns_theta_min         4.279
_exptl_absorpt_coefficient_mu    1.785
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.86780
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.93a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.239
_exptl_crystal_description       block
_exptl_crystal_F_000             1584
_exptl_crystal_size_max          0.255
_exptl_crystal_size_mid          0.213
_exptl_crystal_size_min          0.114
_refine_diff_density_max         0.780
_refine_diff_density_min         -0.439
_refine_diff_density_rms         0.056
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     919
_refine_ls_number_reflns         16059
_refine_ls_number_restraints     14
_refine_ls_restrained_S_all      1.066
_refine_ls_R_factor_all          0.0372
_refine_ls_R_factor_gt           0.0348
_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^)+(0.0472P)^2^+1.8901P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0925
_refine_ls_wR_factor_ref         0.0943
_reflns_Friedel_coverage         0.000
_reflns_number_gt                14862
_reflns_number_total             16059
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3sc05862j2.cif
_cod_data_source_block           s22djl01
_cod_database_code               1570638
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_max   0.822
_shelx_estimated_absorpt_t_min   0.659
_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
 C10-C12 \\sim C10-C12B
 with sigma of 0.02
 C10-C11 \\sim C10-C11B
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C11B \\sim C11 \\sim C12 \\sim C12B: within 2A with sigma of 0.02 and sigma for
terminal atoms of 0.01 within 2A
4. Others
 Fixed Sof: H10(0.55) H10A(0.45) C11(0.55) H11A(0.55) H11B(0.55) H11C(0.55)
 C12(0.55) H12A(0.55) H12B(0.55) H12C(0.55) C11B(0.45) H11D(0.45) H11E(0.45)
 H11F(0.45) C12B(0.45) H12D(0.45) H12E(0.45) H12F(0.45)
5.a Ternary CH refined with riding coordinates:
 C10(H10), C10(H10A), C016(H016), C19(H19), C22(H22), C10A(H10B), C13A(H13A),
 C22A(H22A), C25A(H25A)
5.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C6(H6), C7(H7), C8(H8), C15(H15), C16(H16), C17(H17),
 C26(H26), C27(H27), C28(H28), C29(H29), C30(H30), C32(H32), C33(H33), C34(H34),
  C35(H35), C36(H36), C38(H38), C39(H39), C40(H40), C41(H41), C42(H42),
 C2A(H2A), C3A(H3A), C6A(H6A), C7A(H7A), C8A(H8A), C18A(H18A), C19A(H19A),
 C20A(H20D), C29A(H29A), C30A(H30A), C31A(H31A), C32A(H32A), C33A(H33A),
 C35A(H35A), C36A(H36A), C37A(H37A), C38A(H38A), C39A(H39A), C41A(H41A),
 C42A(H42A), C43A(H43A), C44A(H44A), C45A(H45A)
5.c Idealised Me refined as rotating group:
 C01Q(H01A,H01B,H01C), C02E(H02A,H02B,H02C), C20(H20A,H20B,H20C), C21(H21A,
 H21B,H21C), C23(H23A,H23B,H23C), C24(H24A,H24B,H24C), C11(H11A,H11B,H11C),
 C12(H12A,H12B,H12C), C11B(H11D,H11E,H11F), C12B(H12D,H12E,H12F), C11A(H11G,
 H11H,H11I), C12A(H12G,H12H,H12I), C14A(H14A,H14B,H14C), C15A(H15A,H15B,H15C),
 C23A(H23D,H23E,H23F), C24A(H24D,H24E,H24F), C26A(H26A,H26B,H26C), C27A(H27A,
 H27B,H27C)
;
_shelx_res_checksum              72634
_olex2_submission_special_instructions 'No special instructions were received'