Late transition metal complexes of a new P-N ligand Ph~2~PCH~2~N(H)C~5~H~3~(Cl-5)N: synthesis and structural studies
Coles, Simon J.; Durran, Sean E.; Hursthouse, Michael B.; Slawin, Alexandra M. Z.; Smith, Martin B.; New Journal of Chemistry 25 (2001) 416–422; doi:10.1039/b008502m

data_7051069
_publ_section_title
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 Late transition metal complexes of a new P-N ligand
 Ph~2~PCH~2~N(H)C~5~H~3~(Cl-5)N: synthesis and structural studies
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_journal_issue                   3
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              416
_journal_page_last               422
_journal_paper_doi               10.1039/b008502m
_journal_volume                  25
_journal_year                    2001
_chemical_formula_analytical     'C30 H28 Cl2 N3 P Pd '
_chemical_formula_moiety         'C30 H28 Cl2 N3 P Pd '
_chemical_formula_structural     'C30 H28 Cl2 N3 P Pd '
_chemical_formula_sum            'C30 H28 Cl2 N3 P Pd'
_chemical_formula_weight         638.85
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_cell_angle_alpha                90
_cell_angle_beta                 91.36(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.944(3)
_cell_length_b                   14.623(2)
_cell_length_c                   16.140(2)
_cell_measurement_reflns_used    18
_cell_measurement_temperature    293.2
_cell_measurement_theta_max      8.3
_cell_measurement_theta_min      6.7
_cell_volume                     2818.1(9)
_computing_cell_refinement       'MSC/AFC Diffractometer Control'
_computing_data_collection       'MSC/AFC Diffractometer Control'
_computing_data_reduction        'teXsan (MSC, 1992-1997)'
_computing_publication_material  'teXsan (MSC, 1992-1997)'
_computing_structure_refinement  'teXsan (MSC, 1992-1997)'
_computing_structure_solution    'teXsan (MSC, 1992-1997)'
_diffrn_ambient_temperature      293.2
_diffrn_measurement_device_type  'Rigaku AFC7S'
_diffrn_measurement_method       \w
_diffrn_orient_matrix_UB_11      -0.05330
_diffrn_orient_matrix_UB_12      0.05196
_diffrn_orient_matrix_UB_13      0.00727
_diffrn_orient_matrix_UB_21      -0.04496
_diffrn_orient_matrix_UB_22      -0.03828
_diffrn_orient_matrix_UB_23      0.03832
_diffrn_orient_matrix_UB_31      0.04638
_diffrn_orient_matrix_UB_32      0.02261
_diffrn_orient_matrix_UB_33      0.04816
_diffrn_radiation_detector       'scintillation counter'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'X-ray tube'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.04939
_diffrn_reflns_av_sigmaI/netI    0.100
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            5437
_diffrn_reflns_reduction_process 'Lp corrections applied'
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.52
_diffrn_standards_decay_%        -1.52
_diffrn_standards_interval_count 150
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.920
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.559
_exptl_absorpt_correction_type
;
\y scans (North,Phillips & Matthews, 1968)
;
_exptl_crystal_colour            colourlessprism
_exptl_crystal_density_diffrn    1.506
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1296.00
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.29
_exptl_crystal_size_min          0.16
_exptl_special_details
;
The scan width was (0.89+0.35tan\q)\% with an \w
scan speed of 0\% per minute 
(up to 5 scans to achieve I/\s(I) > 12).
Stationary background counts were recorded at each end of the
scan, and the scan time:background time ratio was 2:1.
;
_refine_diff_density_max         0.55
_refine_diff_density_min         -0.48
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.438
_refine_ls_goodness_of_fit_ref   1.438
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     335
_refine_ls_number_reflns         2869
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0369
_refine_ls_R_factor_gt           0.0369
_refine_ls_shift/esd_max         1.3150
_refine_ls_shift/esd_mean        0.0300
_refine_ls_structure_factor_coef F
_refine_ls_weighting_scheme      'w = 1/[\s^2^(Fo) + 0.00029|Fo|^2^]'
_refine_ls_wR_factor_all         0.0481
_refine_ls_wR_factor_ref         0.0481
_reflns_number_gt                2869
_reflns_number_total             5175
_reflns_threshold_expression     I>3.00\s(I)
_cod_data_source_file            b008502m.txt
_cod_data_source_block           5
_cod_depositor_comments
;
 Adding additional information from the original data file.

 Antanas Vaitkus,
 2017-02-09
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_cod_original_sg_symbol_H-M      'P 21/c'
_cod_original_formula_sum        'C30 H28 Cl2 N3 P Pd '
_cod_database_code               7051069