3H-1,3-Azaphospholo[4,5-b]pyridines - novel heterocyclic P,N-bridging or hybrid ligands: synthesis and first d(8)-transition metal complexes.
Adam, Mohamed Shaker S.; Kindermann, Markus K.; Jones, Peter G.; Heinicke, Joachim W.; Dalton transactions (Cambridge, England : 2003) 45 (2016) 2261–2272; doi:10.1039/c5dt04073f

data_7037447
_publ_section_title
;
 3H-1,3-Azaphospholo[4,5-b]pyridines - novel heterocyclic P,N-bridging or
 hybrid ligands: synthesis and first d(8)-transition metal complexes.
;
_journal_issue                   5
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              2261
_journal_page_last               2272
_journal_paper_doi               10.1039/c5dt04073f
_journal_volume                  45
_journal_year                    2016
_chemical_formula_sum            'C34 H42 Cl4 D12 N4 O2 P2 Pd2'
_chemical_formula_weight         979.43
_chemical_name_systematic
;
 ?
;
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_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
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_atom_sites_solution_secondary   difmap
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_audit_update_record
;
2015-09-08 deposited with the CCDC.
2015-11-24 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 115.816(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.9584(4)
_cell_length_b                   29.4872(8)
_cell_length_c                   13.0738(4)
_cell_measurement_reflns_used    18418
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.6071
_cell_measurement_theta_min      2.6899
_cell_volume                     4150.0(3)
_computing_cell_refinement
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.13 (release 29-11-2007 CrysAlis171 .NET)
(compiled Nov 29 2007,17:23:28)
;
_computing_data_collection
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CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.13 (release 29-11-2007 CrysAlis171 .NET)
(compiled Nov 29 2007,17:23:28)
;
_computing_data_reduction
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.13 (release 29-11-2007 CrysAlis171 .NET)
(compiled Nov 29 2007,17:23:28)
;
_computing_molecular_graphics    'Siemens XP'
_computing_publication_material  SHELXL-97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 16.1057
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Oxford Diffraction Xcalibur S'
_diffrn_measurement_method       \w-scan
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0800
_diffrn_reflns_av_sigmaI/netI    0.0888
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       39
_diffrn_reflns_limit_k_min       -39
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            76588
_diffrn_reflns_theta_full        28.28
_diffrn_reflns_theta_max         28.28
_diffrn_reflns_theta_min         2.70
_exptl_absorpt_coefficient_mu    1.236
_exptl_absorpt_correction_T_max  1.00000
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CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.13 (release 29-11-2007 CrysAlis171 .NET)
(compiled Nov 29 2007,17:23:28)
;
_exptl_crystal_colour            yellow
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_exptl_crystal_description       tablet
_exptl_crystal_F_000             1968
_exptl_crystal_size_max          0.14
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_exptl_crystal_size_min          0.06
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_refine_diff_density_min         -0.474
_refine_diff_density_rms         0.092
_refine_ls_extinction_method     none
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_refine_ls_number_restraints     266
_refine_ls_restrained_S_all      0.814
_refine_ls_R_factor_all          0.0680
_refine_ls_R_factor_gt           0.0304
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0199P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0481
_refine_ls_wR_factor_ref         0.0516
_reflns_number_gt                6543
_reflns_number_total             10287
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5dt04073f3.cif
_cod_data_source_block           shaker
_cod_depositor_comments
;
The following automatic conversions were performed:

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

Automatic conversion script
Id: cif_fix_values 4268 2015-11-12 08:31:59Z antanas 

 Adding full bibliography for 7037445--7037448.cif.
;
_cod_original_cell_volume        4150.0(2)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_original_formula_sum        'C34 H42 D12 Cl4 N4 O2 P2 Pd2'
_cod_database_code               7037447