Chasing the agostic interaction in ligand assisted cyclometallation reactions of palladium (II)
Nielson, A. J.; Harrison, John A.; Sajjad, Arif; Schwerdtfeger, Peter; Rees, Nick; Christensen, Kirsten; Dalton Transactions  (2017) –; doi:10.1039/C7DT03525J

data_7044628
_publ_section_title
;
 Chasing the agostic interaction in ligand assisted cyclometallation
 reactions of palladium (II)
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/C7DT03525J
_journal_year                    2017
_chemical_formula_moiety         'C20 H20 Cl2 N2 O2 Pd2'
_chemical_formula_sum            'C20 H20 Cl2 N2 O2 Pd2'
_chemical_formula_weight         604.10
_chemical_melting_point          ?
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     other
_audit_creation_date             2016-10-10
_audit_creation_method           CRYSTALS_ver_14.43
_audit_update_record
;
2017-07-04 deposited with the CCDC.
2017-11-02 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 99.1931(17)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.6451(1)
_cell_length_b                   17.2164(3)
_cell_length_c                   15.4658(3)
_cell_measurement_reflns_used    12533
_cell_measurement_temperature    150
_cell_measurement_theta_max      76
_cell_measurement_theta_min      4
_cell_volume                     2009.48(6)
_computing_cell_refinement       'CrysAlis, (Oxford Diffraction, 2002)'
_computing_data_collection       'SuperNova, (Oxford Diffraction, 2010)'
_computing_data_reduction        'CrysAlis, (Oxford Diffraction, 2002)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'Superflip (Palatinus & Chapuis, 2007)'
_diffrn_ambient_temperature      150
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device       Area
_diffrn_measurement_device_type  'Oxford Diffraction SuperNova'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.034
_diffrn_reflns_av_sigmaI/netI    0.0420
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            28588
_diffrn_reflns_theta_full        76.205
_diffrn_reflns_theta_max         76.205
_diffrn_reflns_theta_min         3.870
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    17.048
_exptl_absorpt_correction_T_max  0.36
_exptl_absorpt_correction_T_min  0.02
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'CrysAlis, (Oxford Diffraction, 2002)'
_exptl_crystal_colour            lusterous_pale_yellow
_exptl_crystal_density_diffrn    1.997
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1184
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.67
_refine_diff_density_min         -0.86
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.0852
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     260
_refine_ls_number_reflns         2882
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0601
_refine_ls_R_factor_gt           0.0575
_refine_ls_shift/su_max          0.0005471
_refine_ls_shift/su_mean         0.0000235
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method= Modified Sheldrick 
 w=1/[\s^2^(F^2^) + ( 0.12P)^2^ + 0.00P] 
 ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1392
_refine_ls_wR_factor_gt          0.1349
_refine_ls_wR_factor_ref         0.1389
_reflns_limit_h_max              9
_reflns_limit_h_min              -9
_reflns_limit_k_max              21
_reflns_limit_k_min              0
_reflns_limit_l_max              19
_reflns_limit_l_min              0
_reflns_number_gt                2660
_reflns_number_total             4191
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   4.22
_oxford_diffrn_Wilson_scale      0.49
_oxford_refine_ls_r_factor_ref   0.0601
_oxford_refine_ls_scale          1.472(16)
_oxford_reflns_number_all        2883
_oxford_reflns_threshold_expression_ref I>-3.0\s(I)
_oxford_structure_analysis_title 6642
_cod_data_source_file            c7dt03525j2.cif
_cod_data_source_block           A
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value 'not measured' was changed to '?' -
the value is undefined or not given.

'_atom_sites_solution_primary' value 'Other' changed to 'other'
according to
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 4973 2017-02-22 13:04:09Z antanas 
;
_cod_original_sg_symbol_H-M      'P 21/n '
_cod_database_code               7044628
_iucr_refine_instructions_details_constraints
;
BLOCK SCALE X'S 
CONT FIRST(U'S) UNTIL C(21) 
CONT C(24,U'S) UNTIL CL(34) 
EQUIV PART(1001, OCC) PART(1002, OCC) 
WEIGHT -1 PART(1002, OCC) 
RIDE C(22,U'S) C(122,U'S) 
RIDE C(23,U'S) C(123,U'S) 
RIDE C   (   2,X'S) H   (  21,X'S) H   (  22,X'S) 
RIDE C   (   3,X'S) H   (  31,X'S) H   (  32,X'S) 
RIDE C   (   4,X'S) H   (  42,X'S) H   (  41,X'S) 
RIDE C   (   6,X'S) H   (  61,X'S) 
RIDE C   (   7,X'S) H   (  71,X'S) 
RIDE C   (   8,X'S) H   (  81,X'S) 
RIDE O   (  12,X'S) H   ( 121,X'S) 
RIDE C   (  22,X'S) H   ( 221,X'S) H   ( 222,X'S) 
RIDE C   (  23,X'S) H   ( 231,X'S) H   ( 232,X'S) 
RIDE C   ( 122,X'S) H   (1221,X'S) H   (1222,X'S) 
RIDE C   ( 123,X'S) H   (1231,X'S) H   (1232,X'S) 
RIDE C   (  24,X'S) H   ( 242,X'S) H   ( 241,X'S) 
RIDE C   (  26,X'S) H   ( 261,X'S) 
RIDE C   (  27,X'S) H   ( 271,X'S) 
RIDE C   (  28,X'S) H   ( 281,X'S) 
RIDE O   (  32,X'S) H   ( 321,X'S) 
END                                                                             
;
_iucr_refine_instructions_details_restraints
;
NO 
REM   HREST   START (DO NOT REMOVE THIS LINE) 
REM   HREST   END (DO NOT REMOVE THIS LINE) 
END                                                                             
;