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_1570634
_publ_section_title
;
 The structures and reactivity of NHC-supported copper(i) triphenylgermyls
;
_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         'C40 H46 Cu N3 O'
_chemical_formula_sum            'C40 H46 Cu N3 O'
_chemical_formula_weight         648.34
_space_group_crystal_system      orthorhombic
_space_group_IT_number           29
_space_group_name_Hall           'P 2c -2ac'
_space_group_name_H-M_alt        'P c a 21'
_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
;
2023-11-28 deposited with the CCDC.	2023-12-01 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.2264(3)
_cell_length_b                   10.8168(3)
_cell_length_c                   20.4792(7)
_cell_measurement_reflns_used    6998
_cell_measurement_temperature    150.01(10)
_cell_measurement_theta_max      72.3990
_cell_measurement_theta_min      4.0720
_cell_volume                     3594.46(17)
_computing_cell_refinement       'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_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      150.15
_diffrn_detector_area_resol_mean 8.1150
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.990
_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  0.0370
_diffrn_reflns_av_unetI/netI     0.0350
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            23418
_diffrn_reflns_point_group_measured_fraction_full 0.979
_diffrn_reflns_point_group_measured_fraction_max 0.960
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.818
_diffrn_reflns_theta_min         4.087
_exptl_absorpt_coefficient_mu    1.104
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.85567
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.49 (Rigaku Oxford Diffraction, 2022)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.198
_exptl_crystal_description       plank
_exptl_crystal_F_000             1376
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.701
_refine_diff_density_min         -0.363
_refine_diff_density_rms         0.055
_refine_ls_abs_structure_details
;
 Flack x determined using 2354 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.01(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     421
_refine_ls_number_reflns         6888
_refine_ls_number_restraints     91
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0615
_refine_ls_R_factor_gt           0.0522
_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^)+(0.0834P)^2^+1.1881P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1377
_refine_ls_wR_factor_ref         0.1468
_reflns_Friedel_coverage         0.881
_reflns_Friedel_fraction_full    0.957
_reflns_Friedel_fraction_max     0.927
_reflns_number_gt                5954
_reflns_number_total             6888
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3sc05862j2.cif
_cod_data_source_block           s22djl24
_cod_database_code               1570634
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_max   0.968
_shelx_estimated_absorpt_t_min   0.888
_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
 C24-C22 \\sim C24A-C22 \\sim C23A-C22 \\sim C23-C22
 with sigma of 0.005
3. Uiso/Uaniso restraints and constraints
C23 \\sim C24 \\sim C23A \\sim C24A: within 2A with sigma of 0.02 and sigma for
terminal atoms of 0.01 within 2A
O1 \\sim N3 \\sim C28 \\sim C29 \\sim C30 \\sim C31 \\sim C32 \\sim C33 \\sim
C34 \\sim C35 \\sim C40: within 2A with sigma of 0.02 and sigma for terminal
atoms of 0.01 within 2A
4. Others
 Fixed Sof: H22(0.5) H22A(0.5) C23(0.5) H23A(0.5) H23B(0.5) H23C(0.5) C24(0.5)
 H24A(0.5) H24B(0.5) H24C(0.5) C23A(0.5) H23D(0.5) H23E(0.5) H23F(0.5)
 C24A(0.5) H24D(0.5) H24E(0.5) H24F(0.5)
5.a Ternary CH refined with riding coordinates:
 C10(H10), C13(H13), C22(H22), C22(H22A), C25(H25)
5.b Me refined with riding coordinates:
 C24(H24A,H24B,H24C)
5.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C6(H6), C7(H7), C8(H8), C18(H18), C19(H19), C20(H20),
 C29(H29), C30(H30), C31(H31), C32(H32), C33(H33), C40(H40), C39(H39), C38(H38),
  C37(H37), C36(H36)
5.d Fitted hexagon refined as free rotating group:
 C35(C40,C39,C38,C37,C36)
5.e Idealised Me refined as rotating group:
 C11(H11A,H11B,H11C), C12(H12A,H12B,H12C), C14(H14A,H14B,H14C), C15(H15A,H15B,
 H15C), C26(H26A,H26B,H26C), C27(H27A,H27B,H27C), C23(H23A,H23B,H23C),
 C23A(H23D,H23E,H23F), C24A(H24D,H24E,H24F)
;
_shelx_res_checksum              3917
_olex2_submission_special_instructions 'No special instructions were received'