Novel and facile procedure for the synthesis of Ni(II) and Pd(II) PSCOP pincer complexes. Evaluation of their catalytic activity on C-S, C-Se and C-C cross coupling reactions
Valderrama-García, Bianca X.; Rufino-Felipe, Ernesto; Valdés, Hugo; Hernandez-Ortega, Simón; Aguilar-Castillo, Bethsy Adriana; Morales-Morales, David; Inorganica Chimica Acta 502 (2020) 119283–; doi:10.1016/j.ica.2019.119283

data_1565463
_publ_section_title
;
 Novel and facile procedure for the synthesis of Ni(II) and Pd(II) PSCOP
 pincer complexes. Evaluation of their catalytic activity on C-S, C-Se and
 C-C cross coupling reactions
;
_journal_name_full               'Inorganica Chimica Acta'
_journal_page_first              119283
_journal_paper_doi               10.1016/j.ica.2019.119283
_journal_volume                  502
_journal_year                    2020
_chemical_formula_moiety         'C22 H39 Cl Ni O P2 S'
_chemical_formula_sum            'C22 H39 Cl Ni O P2 S'
_chemical_formula_weight         507.69
_space_group_IT_number           9
_space_group_name_Hall           'C -2yc'
_space_group_name_H-M_alt        'C 1 c 1'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'C -2yc'
_symmetry_space_group_name_H-M   'C 1 c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 99.8290(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            20
_cell_length_a                   73.218(6)
_cell_length_b                   7.9782(6)
_cell_length_c                   21.9591(17)
_cell_measurement_reflns_used    9995
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      25.32
_cell_measurement_theta_min      2.31
_cell_volume                     12639.1(17)
_computing_cell_refinement       'SMART V 5.625 (Bruker, 1999)'
_computing_data_collection       'SMART V 5.625 (Bruker, 1999)'
_computing_data_reduction        'SAINT V 7.34A (Bruker, 2006)'
_computing_molecular_graphics    'SHELXTL V 6.12 (Sheldrick, 2000)'
_computing_publication_material  'SHELXTL V 6.12 (Sheldrick, 2000)'
_computing_structure_refinement  'SHELXTL V 6.12 (Sheldrick, 2000)'
_computing_structure_solution    'SHELXTL V 6.12 (Sheldrick, 2000)'
_diffrn_ambient_temperature      123(2)
_diffrn_detector_area_resol_mean 0.661
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Bruker Smart Apex CCD diffractometer 01-670'
_diffrn_measurement_method       \w-scans
_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  0.0488
_diffrn_reflns_av_sigmaI/netI    0.0801
_diffrn_reflns_limit_h_max       88
_diffrn_reflns_limit_h_min       -87
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            36327
_diffrn_reflns_theta_full        25.36
_diffrn_reflns_theta_max         25.36
_diffrn_reflns_theta_min         1.87
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    1.093
_exptl_absorpt_correction_T_max  0.8480
_exptl_absorpt_correction_T_min  0.7015
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(Sheldrick, 2008)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.334
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             5400
_exptl_crystal_size_max          0.392
_exptl_crystal_size_mid          0.322
_exptl_crystal_size_min          0.162
_refine_diff_density_max         1.387
_refine_diff_density_min         -0.573
_refine_diff_density_rms         0.104
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.539(12)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1419
_refine_ls_number_reflns         20770
_refine_ls_number_restraints     337
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0739
_refine_ls_R_factor_gt           0.0612
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0771P)^2^+6.5714P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1367
_refine_ls_wR_factor_ref         0.1446
_reflns_number_gt                17642
_reflns_number_total             20770
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ICA-2020-502-119283.cif
_cod_data_source_block           123MMD10
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_symmetry_cell_setting' value 'Monoclinic' was changed to
'monoclinic' in accordance with the built-in table derived from the
CIF Core dictionary named 'cif_core.dic' version 2.4.5 last updated
on 2014-11-21.

Automatic conversion script
Id: cif_fix_values 8738 2021-04-28 16:35:53Z antanas 
;
_cod_original_sg_symbol_Hall     'c -2yc'
_cod_original_sg_symbol_H-M      'C c'
_cod_database_code               1565463