A Stable Ring-Expanded NHC-Supported Copper Boryl and its Reactivity towards Heterocumulenes
Horsley Downie, Thomas Mardale; Charman, Rex S. C.; Hall, Jonathan W.; Mahon, Mary F.; Lowe, John P.; Liptrot, David Jonathan; Dalton Transactions  (2021) –; doi:10.1039/D1DT03540A

data_7708610
_publ_section_title
;
 A Stable Ring-Expanded NHC-Supported Copper Boryl and its Reactivity
 towards Heterocumulenes
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D1DT03540A
_journal_year                    2021
_chemical_formula_moiety         'C34 H52 B Cu N2 O2'
_chemical_formula_sum            'C37 H59 B Cu N2 O2'
_chemical_formula_weight         638.21
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2020-12-01
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2021-10-19 deposited with the CCDC.	2021-10-21 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 100.7490(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.54170(10)
_cell_length_b                   15.34960(10)
_cell_length_c                   19.7734(2)
_cell_measurement_reflns_used    16986
_cell_measurement_temperature    150.01(10)
_cell_measurement_theta_max      72.9440
_cell_measurement_theta_min      4.5620
_cell_volume                     3739.79(6)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.1150
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.975
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, EosS2'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0203
_diffrn_reflns_av_unetI/netI     0.0177
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.975
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            25521
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.975
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.291
_diffrn_reflns_theta_min         3.587
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.051
_exptl_absorpt_correction_T_max  0.51317
_exptl_absorpt_correction_T_min  0.47071
_exptl_absorpt_correction_type   sphere
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Spherical absorption correction
 using equivalent radius and absorption coefficient.
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    1.134
_exptl_crystal_description       block
_exptl_crystal_F_000             1380
_exptl_crystal_size_max          0.313
_exptl_crystal_size_mid          0.175
_exptl_crystal_size_min          0.13
_exptl_crystal_size_rad          0.251
_refine_diff_density_max         0.343
_refine_diff_density_min         -0.388
_refine_diff_density_rms         0.040
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     373
_refine_ls_number_reflns         7337
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0332
_refine_ls_R_factor_gt           0.0313
_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^)+(0.0500P)^2^+1.0256P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0878
_refine_ls_wR_factor_ref         0.0894
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6826
_reflns_number_total             7337
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt03540a2.cif
_cod_data_source_block           s20djl07-cpd1
_cod_database_code               7708610
_shelxl_version_number           2014-3
_chemical_oxdiff_usercomment     'Colourless blocks'
_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.a Ternary CH refined with riding coordinates:
 C26(H26), C11(H11), C14(H14), C23(H23)
2.b Secondary CH2 refined with riding coordinates:
 C3(H3A,H3B), C2(H2A,H2B), C4(H4A,H4B)
2.c Aromatic/amide H refined with riding coordinates:
 C21(H21), C19(H19), C7(H7), C20(H20), C8(H8), C9(H9)
2.d Idealised Me refined as rotating group:
 C34(H34A,H34B,H34C), C31(H31A,H31B,H31C), C30(H30A,H30B,H30C), C33(H33A,H33B,
 H33C), C12(H12A,H12B,H12C), C13(H13A,H13B,H13C), C27(H27A,H27B,H27C), C25(H25A,
 H25B,H25C), C15(H15A,H15B,H15C), C24(H24A,H24B,H24C), C16(H16A,H16B,H16C),
 C28(H28A,H28B,H28C)
;