Catalytic systems based on nickel(ii) complexes with bis(3,5-dimethylpyrazol-1-yl)methane ‒ impact of PPh3 on the formation of precatalysts and selective dimerization of ethylene
Zubkevich, S. V.; Tuskaev, V. A.; Gagieva, S. Ch.; Pavlov, A. A.; Khrustalev, V. N.; Polyakova, O. V.; Zarubin, D. N.; Kurmaev, D. A.; Kolosov, N. A.; Bulychev, B. M.; New Journal of Chemistry 44 (2020) 981–993; doi:10.1039/C9NJ05704H

data_7059166
_publ_section_title
;
 Catalytic systems based on nickel(ii) complexes with
 bis(3,5-dimethylpyrazol-1-yl)methane -- impact of PPh3 on the formation
 of precatalysts and selective dimerization of ethylene
;
_journal_issue                   3
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              981
_journal_page_last               993
_journal_paper_doi               10.1039/C9NJ05704H
_journal_volume                  44
_journal_year                    2020
_chemical_formula_moiety
'C22 H32 Br N8 Ni, C18 H15 Br3 Ni P, 1.5(C4 H8 O)'
_chemical_formula_sum            'C46 H59 Br4 N8 Ni2 O1.5 P'
_chemical_formula_weight         1215.96
_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   geom
_atom_sites_solution_primary     difmap
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2013
_audit_update_record
;
2019-01-14 deposited with the CCDC.	2019-12-12 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 91.65(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.695(3)
_cell_length_b                   10.158(2)
_cell_length_c                   35.371(7)
_cell_measurement_reflns_used    600
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.0
_cell_measurement_theta_min      3.3
_cell_volume                     5277.7(18)
_computing_cell_refinement       'iMosflm (Battye et al., 2011)'
_computing_data_collection       'Marccd (Doyle, 2011)'
_computing_data_reduction        iMosflm
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2015)'
_computing_publication_material  SHELXTL
_computing_structure_refinement  'SHELXL (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.969
_diffrn_measured_fraction_theta_max 0.961
_diffrn_measurement_device_type  'Rayonix SX165 CCD'
_diffrn_measurement_method       '/f scan'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.80246
_diffrn_reflns_av_R_equivalents  0.1058
_diffrn_reflns_av_unetI/netI     0.0913
_diffrn_reflns_Laue_measured_fraction_full 0.969
_diffrn_reflns_Laue_measured_fraction_max 0.961
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       44
_diffrn_reflns_limit_l_min       -43
_diffrn_reflns_number            40148
_diffrn_reflns_point_group_measured_fraction_full 0.969
_diffrn_reflns_point_group_measured_fraction_max 0.961
_diffrn_reflns_theta_full        28.782
_diffrn_reflns_theta_max         30.981
_diffrn_reflns_theta_min         3.349
_exptl_absorpt_coefficient_mu    5.177
_exptl_absorpt_correction_T_max  0.900
_exptl_absorpt_correction_T_min  0.570
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Scala (Evans, 2006)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.530
_exptl_crystal_description       plate
_exptl_crystal_F_000             2456
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.133
_refine_diff_density_min         -0.853
_refine_diff_density_rms         0.159
_refine_ls_extinction_coef       0.0056(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     595
_refine_ls_number_reflns         11204
_refine_ls_number_restraints     10
_refine_ls_restrained_S_all      1.020
_refine_ls_R_factor_all          0.1097
_refine_ls_R_factor_gt           0.0766
_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^)+(0.0845P)^2^+23.822P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1746
_refine_ls_wR_factor_ref         0.1971
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7873
_reflns_number_total             11204
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9nj05704h2.cif
_cod_data_source_block           6
_cod_depositor_comments
;Adding full bibliography for 7059165--7059166.cif.

 Adding full bibliography for 7059165--7059166.cif.
;
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_original_formula_sum        'C46 H59 Br4 N8 Ni2 O1.50 P'
_cod_database_code               7059166
_shelx_estimated_absorpt_t_min   0.572
_shelx_estimated_absorpt_t_max   0.902
_shelxl_version_number           2013-4
_shelx_res_checksum              42586