Enhanced Catalytic Activity of Nickel Complexes of an Adaptive Diphosphine-Benzophenone Ligand in Alkyne Cyclotrimerization.
Orsino, Alessio F.; Gutiérrez Del Campo, Manuel; Lutz, Martin; Moret, Marc-Etienne; ACS catalysis 9 (2019) 2458–2481; doi:10.1021/acscatal.8b05025

data_4514871
_publ_section_title
;
 Enhanced Catalytic Activity of Nickel Complexes of an Adaptive
 Diphosphine-Benzophenone Ligand in Alkyne Cyclotrimerization.
;
_journal_issue                   3
_journal_name_full               'ACS catalysis'
_journal_page_first              2458
_journal_page_last               2481
_journal_paper_doi               10.1021/acscatal.8b05025
_journal_volume                  9
_journal_year                    2019
_chemical_formula_moiety         'C44 H34 Ni O P2, 1.5(C7 H8)'
_chemical_formula_sum            'C54.5 H46 Ni O P2'
_chemical_formula_weight         837.56
_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   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2016/6
_cell_angle_alpha                102.7809(13)
_cell_angle_beta                 99.4257(13)
_cell_angle_gamma                110.5668(13)
_cell_formula_units_Z            2
_cell_length_a                   10.3659(4)
_cell_length_b                   14.4217(6)
_cell_length_c                   16.3310(7)
_cell_measurement_reflns_used    9915
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.53
_cell_measurement_theta_min      2.18
_cell_volume                     2149.77(16)
_computing_cell_refinement       'SAINT V8.37A'
_computing_data_collection       Apex3
_computing_data_reduction        'SAINT V8.37A, SADABS-2016/2'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_structure_solution    SHELXT
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker Kappa ApexII'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0429
_diffrn_reflns_av_unetI/netI     0.0404
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_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       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            49178
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.536
_diffrn_reflns_theta_min         1.582
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    0.565
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6977
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D.,
 J. Appl. Cryst. 48 (2015) 3-10
;
_exptl_crystal_colour            yellow-orange
_exptl_crystal_density_diffrn    1.294
_exptl_crystal_description       block
_exptl_crystal_F_000             878
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.056
_refine_diff_density_min         -0.482
_refine_diff_density_rms         0.061
_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     528
_refine_ls_number_reflns         9910
_refine_ls_number_restraints     147
_refine_ls_restrained_S_all      1.063
_refine_ls_R_factor_all          0.0611
_refine_ls_R_factor_gt           0.0379
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0425P)^2^+1.4249P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0855
_refine_ls_wR_factor_ref         0.0947
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7704
_reflns_number_total             9910
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cs8b05025_si_002.cif
_cod_data_source_block           l0912a
_cod_original_cell_volume        2149.77(15)
_cod_original_formula_sum        'C54.50 H46 Ni O P2'
_cod_database_code               4514871
_shelx_shelxl_version_number     2016/6
_shelx_res_checksum              9939
_shelx_hkl_checksum              35771