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_7051070
_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     'C18 H16 Cl N2 O P '
_chemical_formula_moiety         'C18 H16 Cl N2 O P '
_chemical_formula_structural     'C18 H16 Cl N2 O P '
_chemical_formula_sum            'C18 H16 Cl N2 O P'
_chemical_formula_weight         342.76
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_cell_angle_alpha                98.90(4)
_cell_angle_beta                 107.85(2)
_cell_angle_gamma                106.17(3)
_cell_formula_units_Z            2
_cell_length_a                   9.226(2)
_cell_length_b                   12.365(6)
_cell_length_c                   8.559(4)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293.2
_cell_measurement_theta_max      18.1
_cell_measurement_theta_min      16.3
_cell_volume                     861.3(6)
_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
;
SIR92 (Altomare, et. al. 1993)
;
_diffrn_ambient_temperature      293.2
_diffrn_measurement_device_type  'Rigaku AFC7S'
_diffrn_measurement_method       \w
_diffrn_orient_matrix_UB_11      -0.04317
_diffrn_orient_matrix_UB_12      -0.03208
_diffrn_orient_matrix_UB_13      0.08343
_diffrn_orient_matrix_UB_21      -0.10771
_diffrn_orient_matrix_UB_22      0.00558
_diffrn_orient_matrix_UB_23      -0.06199
_diffrn_orient_matrix_UB_31      -0.03566
_diffrn_orient_matrix_UB_32      -0.08096
_diffrn_orient_matrix_UB_33      -0.07333
_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  0.01543
_diffrn_reflns_av_sigmaI/netI    0.050
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            3229
_diffrn_reflns_reduction_process 'Lp corrections applied'
_diffrn_reflns_theta_max         25.02
_diffrn_reflns_theta_min         2.59
_diffrn_standards_decay_%        -0.14
_diffrn_standards_interval_count 150
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.316
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.959
_exptl_absorpt_correction_type
;
\y scans (North,Phillips & Matthews, 1968)
;
_exptl_crystal_colour            clear
_exptl_crystal_density_diffrn    1.321
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             356.00
_exptl_crystal_size_max          0.58
_exptl_crystal_size_mid          0.29
_exptl_crystal_size_min          0.23
_exptl_special_details
;
The scan width was (1.05+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         0.21
_refine_diff_density_min         -0.23
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   2.399
_refine_ls_goodness_of_fit_ref   2.399
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     209
_refine_ls_number_reflns         2160
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0342
_refine_ls_R_factor_gt           0.0342
_refine_ls_shift/esd_max         0.0010
_refine_ls_shift/esd_mean        0.0550
_refine_ls_structure_factor_coef F
_refine_ls_weighting_scheme      'w = 1/[\s^2^(Fo) + 0.00001|Fo|^2^]'
_refine_ls_wR_factor_all         0.0332
_refine_ls_wR_factor_ref         0.0332
_reflns_number_gt                2160
_reflns_number_total             3025
_reflns_threshold_expression     I>3.00\s(I)
_cod_data_source_file            b008502m.txt
_cod_data_source_block           2
_cod_depositor_comments
;
 Adding additional information from the original data file.

 Antanas Vaitkus,
 2017-02-09
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_cod_original_formula_sum        'C18 H16 Cl N2 O P '
_cod_database_code               7051070