2-(2'-Pyridyl)-4,6-diphenylphosphinine versus 2-(2'-pyridyl)-4,6-diphenylpyridine: synthesis and characterization of novel Cr(0), Mo(0) and W(0) carbonyl complexes containing chelating P,N and N,N ligands.
de Krom, Iris; Lutz, Martin; Müller, Christian; Dalton transactions (Cambridge, England : 2003) 44 (2015) 10304–10314; doi:10.1039/c5dt01261a

data_7034983
_publ_section_title
;
 2-(2'-Pyridyl)-4,6-diphenylphosphinine versus
 2-(2'-pyridyl)-4,6-diphenylpyridine: synthesis and characterization of
 novel Cr(0), Mo(0) and W(0) carbonyl complexes containing chelating P,N
 and N,N ligands.
;
_journal_issue                   22
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              10304
_journal_page_last               10314
_journal_paper_doi               10.1039/c5dt01261a
_journal_volume                  44
_journal_year                    2015
_chemical_formula_moiety         'C26 H16 N O4 P W'
_chemical_formula_sum            'C26 H16 N O4 P W'
_chemical_formula_weight         621.22
_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_Hall           'P 2c -2n'
_space_group_name_H-M_alt        'P n a 21'
_symmetry_space_group_name_Hall  'P 2c -2n'
_symmetry_space_group_name_H-M   'P n a 21'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2015-03-25 deposited with the CCDC.
2015-05-07 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.7856(4)
_cell_length_b                   18.8326(5)
_cell_length_c                   7.2886(2)
_cell_measurement_reflns_used    9868
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.47
_cell_measurement_theta_min      2.16
_cell_volume                     2166.78(10)
_computing_cell_refinement       'SAINT V7.68A'
_computing_data_collection       Apex2
_computing_data_reduction        'SAINT V7.68A, Sadabs'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker Kappa ApexII'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0186
_diffrn_reflns_av_unetI/netI     0.0098
_diffrn_reflns_laue_measured_fraction_full 1.000
_diffrn_reflns_laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            42028
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.486
_diffrn_reflns_theta_min         1.683
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    5.440
_exptl_absorpt_correction_T_max  0.3461
_exptl_absorpt_correction_T_min  0.1719
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   SADABS-2008/1
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.904
_exptl_crystal_description       block
_exptl_crystal_F_000             1200
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.38
_exptl_crystal_size_min          0.38
_refine_diff_density_max         0.411
_refine_diff_density_min         -0.350
_refine_diff_density_rms         0.050
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   -0.006(5)
_refine_ls_extinction_coef       0.00074(8)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     300
_refine_ls_number_reflns         4970
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.0114
_refine_ls_R_factor_gt           0.0108
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0151P)^2^+0.8667P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0275
_refine_ls_wR_factor_ref         0.0278
_reflns_Friedel_coverage         0.854
_reflns_friedel_fraction_full    0.999
_reflns_friedel_fraction_max     1.000
_reflns_number_gt                4846
_reflns_number_total             4970
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5dt01261a2.cif
_cod_data_source_block           l0131a
_cod_depositor_comments
'Adding full bibliography for 7034982--7034986.cif.'
_cod_database_code               7034983
_shelx_shelxl_version_number     2014/7
_shelx_res_checksum              44698