Direct Observation of β-Chloride Elimination from an Isolable β-Chloroalkyl Complex of Square-Planar Nickel.
Carpenter, Alex E.; McNeece, Andrew J.; Barnett, Brandon R.; Estrada, Alexander L.; Mokhtarzadeh, Charles C.; Moore, Curtis E.; Rheingold, Arnold L.; Perrin, Charles L.; Figueroa, Joshua S.; Journal of the American Chemical Society 136 (2014) 15481–15484; doi:10.1021/ja508956q

data_4122832
_publ_section_title
;
 Direct Observation of \b-Chloride Elimination from an Isolable
 \b-Chloroalkyl Complex of Square-Planar Nickel.
;
_journal_issue                   44
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              15481
_journal_page_last               15484
_journal_paper_doi               10.1021/ja508956q
_journal_volume                  136
_journal_year                    2014
_chemical_formula_moiety         'C64 H74 Cl4 N2 Pd, 1.5(C5 H12)'
_chemical_formula_sum            'C71.5 H92 Cl4 N2 Pd'
_chemical_formula_weight         1227.67
_chemical_name_common            Pd(eta2-C2Cl4)(CNArDipp2)2
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2014-07-09
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2014.06.27 svn.r2953 for OlexSys, GUI svn.r4855)
;
_cell_angle_alpha                90
_cell_angle_beta                 105.5520(17)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.0333(9)
_cell_length_b                   12.9995(8)
_cell_length_c                   29.6350(19)
_cell_measurement_reflns_used    5675
_cell_measurement_temperature    100
_cell_measurement_theta_max      25.261
_cell_measurement_theta_min      2.254
_cell_volume                     6321.7(7)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection       'APEX2 v2013.6-2 (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXT (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.0
_diffrn_detector                 'Bruker APEX-II CCD'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD Area Detector'
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.977
_diffrn_measurement_device       'Kappa Four-Circle Diffractometer'
_diffrn_measurement_device_type  'Bruker APEX II TXS'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'Double Bounce Multilayer Mirrors'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0560
_diffrn_reflns_av_unetI/netI     0.0607
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.977
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            19592
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.977
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.414
_diffrn_reflns_theta_min         1.999
_diffrn_source                   'Micro Focus Rotating Anode'
_diffrn_source_type              'Bruker TXS'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.506
_exptl_absorpt_correction_T_max  0.0916
_exptl_absorpt_correction_T_min  0.0676
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/2 (Bruker,2014) was used for absorption correction.
wR2(int) was 0.1957 before and 0.0397 after correction.
The Ratio of minimum to maximum transmission is 0.7380.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            Colorless
_exptl_crystal_colour_primary    Colorless
_exptl_crystal_density_diffrn    1.290
_exptl_crystal_description       Plate
_exptl_crystal_F_000             2596
_exptl_crystal_size_max          0.067
_exptl_crystal_size_mid          0.063
_exptl_crystal_size_min          0.011
_refine_diff_density_max         0.486
_refine_diff_density_min         -0.456
_refine_diff_density_rms         0.071
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     338
_refine_ls_number_reflns         5698
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.0672
_refine_ls_R_factor_gt           0.0439
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0466P)^2^+6.9225P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0939
_refine_ls_wR_factor_ref         0.1009
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4407
_reflns_number_total             5698
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja508956q_si_002.cif
_cod_data_source_block           JFig1008_sq
_cod_depositor_comments
;
The following automatic conversions were performed:

'_diffrn_radiation_probe' value 'X-ray' changed to 'x-ray' according
to
/home/saulius/struct/COD-crude-data--automatic-downloads/rss-feeds/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2827 2014-09-09 07:05:25Z andrius 

 Adding full bibliography for 4122830--4122832.cif.
;
_cod_original_formula_sum        'C71.50 H92 Cl4 N2 Pd'
_cod_database_code               4122832
_shelxl_version_number           2014-3
_shelx_estimated_absorpt_t_max   0.994
_shelx_estimated_absorpt_t_min   0.967
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C29) = Uanis(C29B)
Uanis(C28B) = Uanis(C28)
3. Others
 Sof(H27)=Sof(C29B)=Sof(H29A)=Sof(H29B)=Sof(H29C)=Sof(C28B)=Sof(H28A)=
 Sof(H28B)=Sof(H28C)=1-FVAR(1)
 Sof(H00T)=Sof(C29)=Sof(H01A)=Sof(H01B)=Sof(H01C)=Sof(C28)=Sof(H01D)=Sof(H01E)=
 Sof(H01F)=FVAR(1)
4.a Ternary CH refined with riding coordinates:
 C30(H30), C18(H18), C15(H15), C27(H00T), C27(H27)
4.b Aromatic/amide H refined with riding coordinates:
 C5(H5), C6(H6), C7(H7), C11(H11), C13(H13), C12(H12), C25(H25), C23(H23),
 C24(H24)
4.c Idealised Me refined as rotating group:
 C20(H20A,H20B,H20C), C19(H19A,H19B,H19C), C16(H16A,H16B,H16C), C31(H31A,H31B,
 H31C), C32(H32A,H32B,H32C), C17(H17A,H17B,H17C), C29(H01A,H01B,H01C), C28(H01D,
 H01E,H01F), C29B(H29A,H29B,H29C), C28B(H28A,H28B,H28C)
;
_shelx_res_checksum              80521
_shelx_hkl_checksum              71532
_shelx_fab_checksum              75199
_olex2_submission_special_instructions 'No special instructions were received'