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_7037446
_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            'C46 H78 Cl4 N4 O4.5 P2 Pd2'
_chemical_formula_weight         1175.66
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_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_method           SHELXL-97
_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                 90.891(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   27.727(3)
_cell_length_b                   16.625(2)
_cell_length_c                   23.302(3)
_cell_measurement_reflns_used    9734
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.47
_cell_measurement_theta_min      2.25
_cell_volume                     10740(2)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_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_measured_fraction_theta_full 0.977
_diffrn_measured_fraction_theta_max 0.976
_diffrn_measurement_device_type  'Bruker APEX2 CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_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  0.0490
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_diffrn_reflns_limit_h_max       38
_diffrn_reflns_limit_h_min       -39
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            153859
_diffrn_reflns_theta_full        30.00
_diffrn_reflns_theta_max         30.03
_diffrn_reflns_theta_min         2.27
_exptl_absorpt_coefficient_mu    0.972
_exptl_absorpt_correction_T_max  0.8679
_exptl_absorpt_correction_T_min  0.7322
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.454
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             4864
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.331
_refine_diff_density_min         -0.684
_refine_diff_density_rms         0.124
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.179
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     585
_refine_ls_number_reflns         15352
_refine_ls_number_restraints     511
_refine_ls_restrained_S_all      1.185
_refine_ls_R_factor_all          0.0782
_refine_ls_R_factor_gt           0.0409
_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^)+(0.0185P)^2^+64.0719P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0803
_refine_ls_wR_factor_ref         0.0982
_reflns_number_gt                11085
_reflns_number_total             15352
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5dt04073f3.cif
_cod_data_source_block           gstaab
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to
/usr/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

'_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        10739(2)
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_original_formula_sum        'C46 H78 Cl4 N4 O4.50 P2 Pd2'
_cod_database_code               7037446