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_1515213
_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         'C38 H42 N6 O12 Pd, 2(C2 H3 N)'
_chemical_formula_sum            'C42 H48 N8 O12 Pd'
_chemical_formula_weight         963.28
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2011-08-16
_audit_creation_method
;
Olex2 1.1
(compiled 2011.08.12 svn.r1921, GUI svn.r3809)
;
_cell_angle_alpha                77.953(4)
_cell_angle_beta                 76.502(5)
_cell_angle_gamma                72.666(5)
_cell_formula_units_Z            1
_cell_length_a                   8.4350(6)
_cell_length_b                   10.2678(5)
_cell_length_c                   13.5105(7)
_cell_measurement_reflns_used    8352
_cell_measurement_temperature    109.9
_cell_measurement_theta_max      32.0420
_cell_measurement_theta_min      3.1330
_cell_volume                     1073.86(11)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
;
_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
;
XL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution
;
XS, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_diffrn_ambient_temperature      109.9
_diffrn_detector_area_resol_mean 16.1450
_diffrn_measured_fraction_theta_full 0.9952
_diffrn_measured_fraction_theta_max 0.906
_diffrn_measurement_details
;
1 omega -54.00 45.00 1.0000 45.0000
omega____ theta____ kappa____ phi______ frames
- -25.1672 77.0000 -180.0000 99

2 omega -44.00 55.00 1.0000 45.0000
omega____ theta____ kappa____ phi______ frames
- 26.4172 -77.0000 -120.0000 99

3 omega 0.00 92.00 1.0000 45.0000
omega____ theta____ kappa____ phi______ frames
- 26.4172 77.0000 90.0000 92

4 omega -40.00 56.00 1.0000 45.0000
omega____ theta____ kappa____ phi______ frames
- 26.4172 -77.0000 -30.0000 96

5 omega -74.00 10.00 1.0000 45.0000
omega____ theta____ kappa____ phi______ frames
- -25.1672 111.0000 37.0000 84

6 omega -98.00 -45.00 1.0000 45.0000
omega____ theta____ kappa____ phi______ frames
- -25.1672 -37.0000 150.0000 53

7 omega -4.00 97.00 1.0000 45.0000
omega____ theta____ kappa____ phi______ frames
- 26.4172 77.0000 -90.0000 101
;
_diffrn_measurement_device_type  'SuperNova, Single source at offset), Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0022528000
_diffrn_orient_matrix_UB_12      -0.0008090000
_diffrn_orient_matrix_UB_13      -0.0527330000
_diffrn_orient_matrix_UB_21      -0.0894833000
_diffrn_orient_matrix_UB_22      0.0148682000
_diffrn_orient_matrix_UB_23      0.0093407000
_diffrn_orient_matrix_UB_31      -0.0051940000
_diffrn_orient_matrix_UB_32      0.0717086000
_diffrn_orient_matrix_UB_33      -0.0109120000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0315
_diffrn_reflns_av_unetI/netI     0.0418
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            16540
_diffrn_reflns_theta_full        30.01
_diffrn_reflns_theta_max         32.08
_diffrn_reflns_theta_min         3.14
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.505
_exptl_absorpt_correction_T_max  0.981
_exptl_absorpt_correction_T_min  0.942
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_crystal_colour            'clear light orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.490
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             498
_exptl_crystal_size_max          0.1827
_exptl_crystal_size_mid          0.1176
_exptl_crystal_size_min          0.042
_refine_diff_density_max         0.749
_refine_diff_density_min         -0.981
_refine_diff_density_rms         0.091
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.078
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     291
_refine_ls_number_reflns         6809
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.078
_refine_ls_R_factor_all          0.0399
_refine_ls_R_factor_gt           0.0367
_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^)+(0.0445P)^2^+0.6314P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0919
_refine_ls_wR_factor_ref         0.0942
_reflns_number_gt                6462
_reflns_number_total             6809
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2sc01050j.txt
_cod_data_source_block           ijsf1110
_cod_database_code               1515213
_chemical_oxdiff_formula         'C22 H23 N3 O6 Pd1'
_chemical_oxdiff_usercomment     'Somia's Hpap-new 2 - NO2'
_reflns_odcompleteness_completeness 99.52
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     30.01