On the appearance of nitrite anion in [PdX(OAc)L2] and [Pd(X)(C^N)L] syntheses (X = OAc or NO2): photocrystallographic identification of metastable Pd(η1-ONO)(C^N)PPh3
Bajwa, Somia E.; Storr, Thomas E.; Hatcher, Lauren E.; Williams, Thomas J.; Baumann, Christoph G.; Whitwood, Adrian C.; Allan, David R.; Teat, Simon J.; Raithby, Paul R.; Fairlamb, Ian J. S.; Chemical Science 3 (2012) 1656–; doi:10.1039/c2sc01050j

data_1515211
_publ_section_title
;
 On the appearance of nitrite anion in [PdX(OAc)L2] and [Pd(X)(C^N)L]
 syntheses (X = OAc or NO2): photocrystallographic identification of
 metastable Pd(\h1-ONO)(C^N)PPh3
;
_journal_issue                   5
_journal_name_full               'Chemical Science'
_journal_page_first              1656
_journal_paper_doi               10.1039/c2sc01050j
_journal_volume                  3
_journal_year                    2012
_chemical_formula_moiety         'C39 H37 Cl2 N2 O6 P Pd'
_chemical_formula_sum            'C39 H37 Cl2 N2 O6 P Pd'
_chemical_formula_weight         837.98
_chemical_name_systematic
;
Nitro-(1-(3,4-dimethoxybenzyl)-6,7-dimethoxyisoquinoline)(triphenylphosphine)
palladium(II)
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/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                 105.4190(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.6878(7)
_cell_length_b                   21.7334(14)
_cell_length_c                   16.3349(10)
_cell_measurement_reflns_used    9928
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      33.58
_cell_measurement_theta_min      2.97
_cell_volume                     3657.7(4)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    WINGX
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  synchrotron
_diffrn_radiation_source         synchrotron
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.7749
_diffrn_reflns_av_R_equivalents  0.0793
_diffrn_reflns_av_sigmaI/netI    0.0755
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            39140
_diffrn_reflns_theta_full        33.64
_diffrn_reflns_theta_max         33.64
_diffrn_reflns_theta_min         2.97
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.747
_exptl_absorpt_correction_T_max  0.9852
_exptl_absorpt_correction_T_min  0.9290
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS V2008-1, Bruker AXS.: Madison, WI, USA, 2008
;
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    1.522
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Plate
_exptl_crystal_F_000             1712
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.622
_refine_diff_density_min         -1.240
_refine_diff_density_rms         0.154
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     477
_refine_ls_number_reflns         11046
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.071
_refine_ls_R_factor_all          0.0563
_refine_ls_R_factor_gt           0.0472
_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^)+(0.0570P)^2^+0.7884P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1207
_refine_ls_wR_factor_ref         0.1262
_reflns_number_gt                9181
_reflns_number_total             11046
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2sc01050j.txt
_cod_data_source_block           150K
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               1515211