Synthesis of 1,3-azaphosphol-2-ones. Crystal and molecular structures of [SP-4-2]-dichlorobis(3-phenyl-1,3-dihydrobenzo[1,3]azaphosphol-2-one-P)palladium(II) and its chloro(methyl)platinum(II) analogue.
Bennett, Justine; Doyle, Roy J.; Lee, Hwi-Young; Lu, Di; Salem, Geoffrey; Speldewinde, David J.; Tifan, Michelle; Willis, Anthony C.; Dalton transactions (Cambridge, England : 2003) 39 (2010) 256–264; doi:10.1039/b916913j

data_7024435
_publ_section_title
;
 Synthesis of 1,3-azaphosphol-2-ones. Crystal and molecular structures of
 [SP-4-2]-dichlorobis(3-phenyl-1,3-dihydrobenzo[1,3]azaphosphol-2-one-P)palladium(II)
 and its chloro(methyl)platinum(II) analogue.
;
_journal_issue                   1
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              256
_journal_page_last               264
_journal_paper_doi               10.1039/b916913j
_journal_volume                  39
_journal_year                    2010
_chemical_compound_source        local
_chemical_formula_moiety
'C26 H20 Cl2 N2 O2 P2 Pd, 1.66(C H4 O), 1.34(H2 O)'
_chemical_formula_sum            'C27.66 H29.32 Cl2 N2 O5 P2 Pd'
_chemical_formula_weight         709.02
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             07-11-22
_audit_creation_method           CRYSTALS_ver_12.18
_audit_update_record
;
2007-11-22 - Report on C27.66 H24 Cl2 N2 O5.00 P2 Pd1
by Anthony C. Willis
for Geoff Salem, Roy Doyle and ?????

2007-11-22 - passes checkcif tests with warnings

;
_cell_angle_alpha                81.4299(12)
_cell_angle_beta                 83.0012(16)
_cell_angle_gamma                77.0439(16)
_cell_formula_units_Z            2
_cell_length_a                   8.6093(2)
_cell_length_b                   11.3301(3)
_cell_length_c                   16.3435(5)
_cell_measurement_reflns_used    46880
_cell_measurement_temperature    200
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      2.6
_cell_volume                     1529.80(7)
_computing_cell_refinement       'Denzo/Scalepack (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius BV, 1997)'
_computing_data_reduction        'Denzo/Scalepack (Otwinowski & Minor, 1997)'
_computing_molecular_graphics
;
ORTEP-II (Johnson 1976) in teXsan (MSC, 1992-1997)
;
_computing_publication_material  'CRYSTALS (Watkin et al 2003)'
_computing_structure_refinement  'CRYSTALS (Watkin et al 2003)'
_computing_structure_solution    'SIR92 (Altomare et al, 1994)'
_diffrn_ambient_temperature      200
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       ' \f and \w scans with CCD '
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.043
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            34432
_diffrn_reflns_theta_full        27.529
_diffrn_reflns_theta_max         27.529
_diffrn_reflns_theta_min         2.642
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.924
_exptl_absorpt_correction_T_max  0.969
_exptl_absorpt_correction_T_min  0.794
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details
;
via Gaussian method (Coppens, 1970) implemented in maXus (2000)
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.528
_exptl_crystal_density_meas      ?
_exptl_crystal_description       needle
_exptl_crystal_F_000             718.55
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.69
_refine_diff_density_min         -0.58
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.1131
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     400
_refine_ls_number_reflns         4819
_refine_ls_number_restraints     38
_refine_ls_R_factor_all          0.0489
_refine_ls_R_factor_gt           0.0284
_refine_ls_shift/su_max          0.027645
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details
;
Method, part 1, Chebychev polynomial,
(Watkin, 1994, Prince, 1982)
[weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)]
where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax
Method = Robust Weighting (Prince, 1982)
W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^
A~i~ are:
0.873 0.175 0.655
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0411
_refine_ls_wR_factor_gt          0.0334
_refine_ls_wR_factor_ref         0.0334
_reflns_limit_h_max              11
_reflns_limit_h_min              -11
_reflns_limit_k_max              14
_reflns_limit_k_min              -14
_reflns_limit_l_max              21
_reflns_limit_l_min              0
_reflns_number_gt                4819
_reflns_number_total             7035
_reflns_threshold_expression     I>3.0\s(I)
_oxford_diffrn_Wilson_B_factor   2.21
_oxford_diffrn_Wilson_scale      8.07
_oxford_refine_ls_scale          0.3725(4)
_oxford_structure_analysis_title '10151247 sal0701'
_cod_data_source_file            b916913j.txt
_cod_data_source_block           sal0701
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_sg_symbol_H-M      'P -1 '
_cod_database_code               7024435