Pyrazole-Based PCN Pincer Complexes of Palladium(II): Mono- and Dinuclear Hydroxide Complexes and Ligand Rollover C‒H Activation
Bailey, Wilson D.; Luconi, Lapo; Rossin, Andrea; Yakhvarov, Dmitry; Flowers, Sarah E.; Kaminsky, Werner; Kemp, Richard A.; Giambastiani, Giuliano; Goldberg, Karen I.; Organometallics 34 (2015) 3998–; doi:10.1021/acs.organomet.5b00355

data_4086137
_publ_section_title
;
 Pyrazole-Based PCN Pincer Complexes of Palladium(II): Mono- and Dinuclear
 Hydroxide Complexes and Ligand Rollover C--H Activation
;
_journal_issue                   16
_journal_name_full               Organometallics
_journal_page_first              3998
_journal_paper_doi               10.1021/acs.organomet.5b00355
_journal_volume                  34
_journal_year                    2015
_chemical_absolute_configuration unk
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C36 H52 B1 Cl F4 N4 P2 Pd2,2(C H2 Cl2)'
_chemical_formula_sum            'C38 H56 B Cl5 F4 N4 P2 Pd2'
_chemical_formula_weight         1107.67
_space_group_IT_number           33
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      33
_symmetry_space_group_name_Hall  'P 2c -2n'
_symmetry_space_group_name_H-M   'P n a 21'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2015-01-28T17:33:32-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   30.989(2)
_cell_length_b                   12.597(10)
_cell_length_c                   11.852(9)
_cell_measurement_reflns_used    3026
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      26.8087
_cell_measurement_theta_min      4.153
_cell_measurement_wavelength     0.71073
_cell_volume                     4627(5)
_computing_cell_refinement
;
        CrysAlisPro, Oxford Diffraction Ltd.,
        Version 1.171.34.41 (release 13-09-2010 CrysAlis171 .NET)
        (compiled Sep 13 2010,14:28:38)
;
_computing_data_collection
;
        CrysAlisPro, Oxford Diffraction Ltd.,
        Version 1.171.34.41 (release 13-09-2010 CrysAlis171 .NET)
        (compiled Sep 13 2010,14:28:38)
;
_computing_data_reduction
;
        CrysAlisPro, Oxford Diffraction Ltd.,
        Version 1.171.34.41 (release 13-09-2010 CrysAlis171 .NET)
        (compiled Sep 13 2010,14:28:38)
;
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-2014/6 (Sheldrick, 2014)'
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean 16.4547
_diffrn_measured_fraction_theta_full 0.971
_diffrn_measured_fraction_theta_max 0.862
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0226311
_diffrn_orient_matrix_UB_12      -0.002137
_diffrn_orient_matrix_UB_13      -0.0091368
_diffrn_orient_matrix_UB_21      0.0015865
_diffrn_orient_matrix_UB_22      0.0550917
_diffrn_orient_matrix_UB_23      0.0113276
_diffrn_orient_matrix_UB_31      0.0032071
_diffrn_orient_matrix_UB_32      -0.0111458
_diffrn_orient_matrix_UB_33      0.0580545
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.1177
_diffrn_reflns_av_unetI/netI     0.277
_diffrn_reflns_Laue_measured_fraction_full 0.971
_diffrn_reflns_Laue_measured_fraction_max 0.862
_diffrn_reflns_limit_h_max       38
_diffrn_reflns_limit_h_min       -34
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            21117
_diffrn_reflns_point_group_measured_fraction_full 0.84
_diffrn_reflns_point_group_measured_fraction_max 0.725
_diffrn_reflns_theta_full        25
_diffrn_reflns_theta_max         26.865
_diffrn_reflns_theta_min         4.161
_exptl_absorpt_coefficient_mu    1.184
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.96846
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
        CrysAlisPro, Oxford Diffraction Ltd.,
        Version 1.171.34.41 (release 13-09-2010 CrysAlis171 .NET)
        (compiled Sep 13 2010,14:28:38)
        Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.59
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2240
_exptl_crystal_size_max          0.03
_exptl_crystal_size_mid          0.01
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.943
_refine_diff_density_min         -0.703
_refine_diff_density_rms         0.167
_refine_ls_abs_structure_details
;
 Flack x determined using 1291 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.03(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.03
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     517
_refine_ls_number_reflns         7191
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.03
_refine_ls_R_factor_all          0.1417
_refine_ls_R_factor_gt           0.0703
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0380P)^2^+0.1969P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1102
_refine_ls_wR_factor_ref         0.1441
_reflns_number_gt                4391
_reflns_number_total             7191
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om5b00355_si_003.cif
_cod_data_source_block           6a
_cod_depositor_comments
'Adding full bibliography for 4086135--4086143.cif.'
_cod_original_cell_volume        4627(8)
_cod_original_formula_sum        'C38 H56 B1 Cl5 F4 N4 P2 Pd2'
_cod_database_code               4086137