Phosphine-functionalized NHC Ni(II) and Ni(0) complexes: synthesis, characterization and catalytic properties
Rull, Silvia; Rama, Raquel J.; Álvarez, Eleuterio; Fructos, Manuel R.; Belderrain, Tomas R.; Nicasio, M. Carmen; Dalton Trans.  (2017) –; doi:10.1039/C7DT01805C

data_7043060
_publ_section_title
;
 Phosphine-functionalized NHC Ni(II) and Ni(0) complexes: synthesis,
 characterization and catalytic properties
;
_journal_name_full               'Dalton Trans.'
_journal_paper_doi               10.1039/C7DT01805C
_journal_year                    2017
_chemical_formula_moiety         'C37 H45 N2 Ni O4 P'
_chemical_formula_sum            'C37 H45 N2 Ni O4 P'
_chemical_formula_weight         671.43
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2016/6
_audit_update_record
;
2017-02-21 deposited with the CCDC.
2017-05-22 downloaded from the CCDC.
;
_cell_angle_alpha                83.689(2)
_cell_angle_beta                 82.032(2)
_cell_angle_gamma                79.558(2)
_cell_formula_units_Z            2
_cell_length_a                   8.7746(4)
_cell_length_b                   11.0588(5)
_cell_length_c                   18.2168(8)
_cell_measurement_reflns_used    6696
_cell_measurement_temperature    213(2)
_cell_measurement_theta_max      23.48
_cell_measurement_theta_min      2.38
_cell_volume                     1715.10(13)
_computing_cell_refinement       'APEX2 Software Suite (Bruker, 2007)'
_computing_data_collection       'APEX2 Software Suite (Bruker, 2007)'
_computing_data_reduction        'APEX2 Software Suite (Bruker, 2007)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL and publCIF (Westrip, 2010)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_structure_solution    'SIR2002 (Burla et al., 2003)'
_diffrn_ambient_temperature      213(2)
_diffrn_detector_area_resol_mean 8.26
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type
;
 Bruker-Nonius X8kappa APEX II CCD area detector
;
_diffrn_measurement_method       'phi and omega scans with narrow frames'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0450
_diffrn_reflns_av_unetI/netI     0.0397
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            32713
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.245
_diffrn_reflns_theta_min         2.278
_exptl_absorpt_coefficient_mu    0.653
_exptl_absorpt_correction_T_max  0.9375
_exptl_absorpt_correction_T_min  0.8804
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
program SADABS, Bruker (2001).
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.300
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             712
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.100
_refine_diff_density_max         0.754
_refine_diff_density_min         -0.476
_refine_diff_density_rms         0.058
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     412
_refine_ls_number_reflns         6194
_refine_ls_number_restraints     35
_refine_ls_restrained_S_all      1.099
_refine_ls_R_factor_all          0.0570
_refine_ls_R_factor_gt           0.0393
_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^)+(0.0657P)^2^+0.4862P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1056
_refine_ls_wR_factor_ref         0.1130
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4883
_reflns_number_total             6194
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt01805c2.cif
_cod_data_source_block           2b
_cod_database_code               7043060
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_min   0.880
_shelx_estimated_absorpt_t_max   0.938
_shelx_res_checksum              20246