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_1515214
_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         'C40 H38 N O6 P Pd, C H2 Cl2'
_chemical_formula_sum            'C41 H40 Cl2 N O6 P Pd'
_chemical_formula_weight         851.01
_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             2011-01-24
_audit_creation_method
;
Olex2 1.1
(compiled 2011.01.21 svn.r1625, GUI svn.r3464)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 107.608(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   47.4181(14)
_cell_length_b                   11.0136(3)
_cell_length_c                   17.7382(6)
_cell_measurement_reflns_used    23218
_cell_measurement_temperature    110.15
_cell_measurement_theta_max      24.9737
_cell_measurement_theta_min      2.9037
_cell_volume                     8829.7(5)
_computing_cell_refinement
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET)
(compiled Oct 25 2010,18:11:34)
;
_computing_data_collection
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET)
(compiled Oct 25 2010,18:11:34)
;
_computing_data_reduction
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET)
(compiled Oct 25 2010,18:11:34)
;
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution
'A short history of SHELX (Sheldrick, 2007)/Bruker'
_diffrn_ambient_temperature      110.15
_diffrn_detector_area_resol_mean 16.1450
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_details
;
1 omega -87.00 4.50 0.7500 5.0000
omega____ theta____ kappa____ phi______ frames
- -17.6138 -37.0000 60.0000 122

2 omega -38.00 -11.00 0.7500 5.0000
omega____ theta____ kappa____ phi______ frames
- -17.6138 142.0000 -133.0000 36

3 omega -88.00 5.00 0.7500 5.0000
omega____ theta____ kappa____ phi______ frames
- -17.6138 -77.0000 -180.0000 124

4 omega -88.00 -7.00 0.7500 5.0000
omega____ theta____ kappa____ phi______ frames
- -17.6138 -77.0000 -30.0000 108

5 omega -77.00 -5.00 0.7500 5.0000
omega____ theta____ kappa____ phi______ frames
- -17.6138 128.0000 -124.0000 96

6 omega -51.00 48.00 0.7500 5.0000
omega____ theta____ kappa____ phi______ frames
- 18.8638 -77.0000 60.0000 132

7 omega -54.00 45.00 0.7500 5.0000
omega____ theta____ kappa____ phi______ frames
- 18.8638 -37.0000 120.0000 132
;
_diffrn_measurement_device_type  'SuperNova, Single source at offset), Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0148643000
_diffrn_orient_matrix_UB_12      -0.0122507000
_diffrn_orient_matrix_UB_13      0.0220963000
_diffrn_orient_matrix_UB_21      -0.0049201000
_diffrn_orient_matrix_UB_22      -0.0281738000
_diffrn_orient_matrix_UB_23      0.0296381000
_diffrn_orient_matrix_UB_31      -0.0007814000
_diffrn_orient_matrix_UB_32      -0.0563894000
_diffrn_orient_matrix_UB_33      -0.0196742000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0332
_diffrn_reflns_av_unetI/netI     0.0240
_diffrn_reflns_limit_h_max       56
_diffrn_reflns_limit_h_min       -56
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            42881
_diffrn_reflns_theta_full        25.11
_diffrn_reflns_theta_max         25.11
_diffrn_reflns_theta_min         2.92
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.619
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.83682
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET)
(compiled Oct 25 2010,18:11:34)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_density_diffrn    1.280
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3488
_exptl_crystal_size_max          0.336
_exptl_crystal_size_mid          0.2842
_exptl_crystal_size_min          0.2773
_platon_squeeze_details
;
;
_refine_diff_density_max         1.292
_refine_diff_density_min         -0.427
_refine_diff_density_rms         0.082
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.095
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     474
_refine_ls_number_reflns         7832
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.095
_refine_ls_R_factor_all          0.0407
_refine_ls_R_factor_gt           0.0373
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0508P)^2^+29.4470P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1018
_refine_ls_wR_factor_ref         0.1038
_reflns_number_gt                7088
_reflns_number_total             7832
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2sc01050j.txt
_cod_data_source_block           ijf1042
_cod_database_code               1515214
_chemical_oxdiff_formula         'C40 H38 N O6 P Pd'
_chemical_oxdiff_usercomment     'Somia's B-19(a)'
_reflns_odcompleteness_completeness 99.73
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     24.97