Direct metal-carbon bonding in symmetric bis(C-H) agostic Nickel(I) complexes
He, Weiying; Beattie, D. Dawson; Zhou, Hao; Bowes, Eric G.; Schafer, Laurel L.; Love, Jennifer; Kennepohl, Pierre; Chemical Science  (2021) –; doi:10.1039/D1SC03578A

data_1565128
_publ_section_title
;
 Direct metal-carbon bonding in symmetric bis(C-H) agostic Nickel(I)
 complexes
;
_journal_name_full               'Chemical Science'
_journal_paper_doi               10.1039/D1SC03578A
_journal_year                    2021
_chemical_formula_moiety         'C36 H40 Cu N3, C4 H8 O'
_chemical_formula_sum            'C40 H48 Cu N3 O'
_chemical_formula_weight         650.35
_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   mixed
_audit_block_doi                 10.5517/ccdc.csd.cc23454l
_audit_creation_method           SHELXL-2017/1
_audit_update_record
;
2019-08-03 deposited with the CCDC.	2021-10-29 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 94.780(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.7832(11)
_cell_length_b                   12.9552(12)
_cell_length_c                   22.918(2)
_cell_measurement_reflns_used    9645
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.31
_cell_measurement_theta_min      2.34
_cell_volume                     3486.3(6)
_computing_cell_refinement       'SAINT V8.37A (Bruker, 2005)'
_computing_data_collection       'APEX3 V2016.5-0 (Bruker, 2016)'
_computing_data_reduction
; 
SAINT V8.37A, XPREP v2014/2, SADABS V2016/2 (Bruker, 2016) 
;
_computing_molecular_graphics    'SHELXLE v932 (Hubschle, 2011)'
_computing_publication_material  'XCIF V2014-2 (Bruker, 2014)'
_computing_structure_refinement  'SHELX-2018-1 (Sheldrick, 2015)'
_computing_structure_solution    'SHELX-2014-5 (Sheldrick, 2015)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device       'Bruker D8 Quest/Photon 100'
_diffrn_measurement_method       'profile data from \f and \w scans'
_diffrn_radiation_monochromator  'multilayer mirrors'
_diffrn_radiation_source         'microfocus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0785
_diffrn_reflns_av_unetI/netI     0.0356
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            119401
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.684
_diffrn_reflns_theta_min         2.341
_exptl_absorpt_coefficient_mu    0.661
_exptl_absorpt_correction_T_max  0.92752
_exptl_absorpt_correction_T_min  0.85285
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2016/2 (Bruker, 2016)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.239
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1384
_exptl_crystal_size_max          0.361
_exptl_crystal_size_mid          0.306
_exptl_crystal_size_min          0.144
_refine_diff_density_max         0.979
_refine_diff_density_min         -0.903
_refine_diff_density_rms         0.082
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     417
_refine_ls_number_reflns         10763
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0626
_refine_ls_R_factor_gt           0.0433
_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^)+(0.0632P)^2^+2.4081P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1104
_refine_ls_wR_factor_ref         0.1236
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8417
_reflns_number_total             10763
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1sc03578a2.cif
_cod_data_source_block           Me3NNCu_NHCPh2_a
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               1565128
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_min   0.796
_shelx_estimated_absorpt_t_max   0.911
_shelx_res_checksum              3318
_shelx_hkl_checksum              14779