Transition metal complexes of the pyridylphosphine ligand o-C6H4(CH2PPy2)2.
Vaughan, Teresa F.; Spencer, John L.; Dalton transactions (Cambridge, England : 2003) 45 (2016) 16826–16837; doi:10.1039/c6dt02041k

data_7040763
_publ_section_title
;
 Transition metal complexes of the pyridylphosphine ligand
 o-C6H4(CH2PPy2)2.
;
_journal_issue                   42
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              16826
_journal_page_last               16837
_journal_paper_doi               10.1039/c6dt02041k
_journal_volume                  45
_journal_year                    2016
_chemical_formula_moiety         'C28 H24 Cl2 N4 P2 Pd,2(C H2 Cl2)'
_chemical_formula_sum            'C30 H28 Cl6 N4 P2 Pd'
_chemical_formula_weight         655.75
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date
;
'Fri Nov 30 08:50:53 2012'
;
_audit_creation_method
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET)
(compiled Sep 14 2012,17:21:16)
;
_audit_update_record
;
2016-08-31 deposited with the CCDC.
2016-09-07 downloaded from the CCDC.
;
_cell_angle_alpha                90.0
_cell_angle_beta                 90.1316(15)
_cell_angle_gamma                90.0
_cell_formula_units_Z            4
_cell_length_a                   14.43316(19)
_cell_length_b                   10.2502(2)
_cell_length_c                   22.5901(5)
_cell_measurement_reflns_used    16224
_cell_measurement_temperature    120.01(10)
_cell_measurement_theta_max      37.6894
_cell_measurement_theta_min      2.6780
_cell_volume                     3342.03(11)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET)
(compiled Sep 14 2012,17:21:16)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET)
(compiled Sep 14 2012,17:21:16)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET)
(compiled Sep 14 2012,17:21:16)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      120.01(10)
_diffrn_detector_area_resol_mean 10.6501
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details
;
  1 omega  -50.00   35.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -       31.9365  -19.0000  -60.0000 85

  2 omega  -44.00   57.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -       31.9365  -77.0000 -150.0000 101

  3 omega -107.00  -74.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      -32.8740  178.0000 -150.0000 33

  4 omega -116.00  -58.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      -32.8740 -178.0000   60.0000 58

  5 omega    2.00   72.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -       31.9365   57.0000  -60.0000 70
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0131249000
_diffrn_orient_matrix_UB_12      0.0326457000
_diffrn_orient_matrix_UB_13      0.0264191000
_diffrn_orient_matrix_UB_21      -0.0271676000
_diffrn_orient_matrix_UB_22      -0.0442352000
_diffrn_orient_matrix_UB_23      0.0167488000
_diffrn_orient_matrix_UB_31      0.0387702000
_diffrn_orient_matrix_UB_32      -0.0420147000
_diffrn_orient_matrix_UB_33      0.0028673000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0367
_diffrn_reflns_av_unetI/netI     0.0562
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            43939
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.999
_diffrn_reflns_theta_min         2.683
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.886
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.59016
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET)
(compiled Sep 14 2012,17:21:16)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear pale yellow'
_exptl_crystal_density_diffrn    1.303
_exptl_crystal_description       block
_exptl_crystal_F_000             1320
_exptl_crystal_recrystallization_method
'vapour diffusion of hexane into a CH2Cl2 solution'
_exptl_crystal_size_max          0.4600
_exptl_crystal_size_mid          0.3400
_exptl_crystal_size_min          0.1900
_refine_diff_density_max         2.740
_refine_diff_density_min         -1.600
_refine_diff_density_rms         0.144
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     334
_refine_ls_number_reflns         9753
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.0623
_refine_ls_R_factor_gt           0.0538
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0753P)^2^+12.1904P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1497
_refine_ls_wR_factor_ref         0.1566
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8312
_reflns_number_total             9753
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt02041k2.cif
_cod_data_source_block           tvanrmo
_cod_depositor_comments
'Adding full bibliography for 7040761--7040764.cif.'
_cod_original_cell_volume        3342.02(11)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7040763
_chemical_oxdiff_formula         C28N24N4P2Cl2Pd1
_cell_oxdiff_angle_alpha         90.029(2)
_cell_oxdiff_angle_beta          90.107(2)
_cell_oxdiff_angle_gamma         90.022(2)
_cell_oxdiff_length_a            14.4381(4)
_cell_oxdiff_length_b            10.2510(3)
_cell_oxdiff_length_c            22.5806(7)
_cell_oxdiff_measurement_reflns_used 16224
_cell_oxdiff_volume              3342.02(16)
_reflns_odcompleteness_completeness 99.92
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     36.23
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C8(H8A,H8B), C1(H1A,H1B)
2.b Aromatic/amide H refined with riding coordinates:
 C13(H13), C3(H3), C0BA(H0BA), C14(H14), C16(H16), C20(H20), C5(H5), C4(H4),
 C10(H10), C22(H22), C15(H15), C2AA(H2AA), C21(H21), C18(H18), C19(H19), C6(H6),
  C24(H24), C26(H26), C23(H23), C25(H25)
;
_shelx_res_checksum              84930
_shelx_fab_checksum              7788
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'