Synthesis and Reactivity of Cyclic (Alkyl)(Amino)Carbene Stabilized Nickel Carbonyl Complexes
Paul, Ursula S. D.; Radius, Udo; Organometallics 36 (2017) 1398–; doi:10.1021/acs.organomet.7b00109

data_4087324
_publ_section_title
;
 Synthesis and Reactivity of Cyclic (Alkyl)(Amino)Carbene Stabilized
 Nickel Carbonyl Complexes
;
_journal_issue                   7
_journal_name_full               Organometallics
_journal_page_first              1398
_journal_paper_doi               10.1021/acs.organomet.7b00109
_journal_volume                  36
_journal_year                    2017
_chemical_formula_moiety         'C25 H40 Br N Ni'
_chemical_formula_sum            'C25 H40 Br N Ni'
_chemical_formula_weight         493.20
_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'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/6
_cell_angle_alpha                90
_cell_angle_beta                 98.366(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.7904(9)
_cell_length_b                   15.2337(13)
_cell_length_c                   14.7013(13)
_cell_measurement_reflns_used    9949
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.07
_cell_measurement_theta_min      2.33
_cell_volume                     2390.9(4)
_computing_cell_refinement       'Saint-NT v. 7.23'
_computing_data_collection       'APEX2 ver. 2014.1 (Bruker AXS)'
_computing_data_reduction        'Saint-NT v. 7.23'
_computing_molecular_graphics    'XP ver. 5.1 (Bruker AXS, 1998)'
_computing_publication_material  'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/6 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXL-2014 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker X8-APEX II'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  helios
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0333
_diffrn_reflns_av_unetI/netI     0.0272
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            22678
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         26.104
_diffrn_reflns_theta_min         1.936
_exptl_absorpt_coefficient_mu    2.493
_exptl_absorpt_correction_T_max  0.7453
_exptl_absorpt_correction_T_min  0.5956
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   'Sadabs 2014/3 (Bruker 2014)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.370
_exptl_crystal_description       block
_exptl_crystal_F_000             1040
_exptl_crystal_size_max          0.142
_exptl_crystal_size_mid          0.117
_exptl_crystal_size_min          0.097
_refine_diff_density_max         0.912
_refine_diff_density_min         -0.591
_refine_diff_density_rms         0.080
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.150
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     302
_refine_ls_number_reflns         4728
_refine_ls_number_restraints     68
_refine_ls_restrained_S_all      1.143
_refine_ls_R_factor_all          0.0538
_refine_ls_R_factor_gt           0.0410
_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^)+(0.0243P)^2^+6.0063P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0896
_refine_ls_wR_factor_ref         0.0963
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3982
_reflns_number_total             4728
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om7b00109_si_002.cif
_cod_data_source_block           compound_5b
_cod_database_code               4087324
_shelx_estimated_absorpt_t_min   0.718
_shelx_estimated_absorpt_t_max   0.794
_shelxl_version_number           2014/6
_shelx_res_checksum              47791
_shelx_hkl_checksum              78624