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_7024436
_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         'C33 H39 Cl N2 O4 P2 Pt'
_chemical_formula_sum            'C33 H36 Cl N2 O4 P2 Pt'
_chemical_formula_weight         820.17
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yab'
_symmetry_space_group_name_H-M   'P 1 21/a 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             07-09-12
_audit_creation_method           CRYSTALS_ver_12.18
_audit_update_record
;
2007-09-17 - Report on C71 H83 C33 H39 Cl N2 O4 P2 Pt
by Anthony C. Willis
for Geoff Salem, Roy Doyle and Justine Bennett

2007-09-17 - passes checkcif tests with minor warnings

;
_cell_angle_alpha                90
_cell_angle_beta                 113.4788(9)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.4641(2)
_cell_length_b                   12.9680(2)
_cell_length_c                   18.4124(3)
_cell_measurement_reflns_used    52649
_cell_measurement_temperature    200
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      2.6
_cell_volume                     3386.69(9)
_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 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.041
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            69517
_diffrn_reflns_theta_full        27.481
_diffrn_reflns_theta_max         27.481
_diffrn_reflns_theta_min         2.635
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.37
_exptl_absorpt_correction_T_max  0.803
_exptl_absorpt_correction_T_min  0.347
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details
;
via Gaussian method (Coppens, 1970) implemented in maXus (2000)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.609
_exptl_crystal_density_meas      ?
_exptl_crystal_description       needle
_exptl_crystal_F_000             1626
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.93
_refine_diff_density_min         -0.83
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.0991
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     395
_refine_ls_number_reflns         5069
_refine_ls_number_restraints     5
_refine_ls_R_factor_all          0.0435
_refine_ls_R_factor_gt           0.0256
_refine_ls_shift/su_max          0.010060
_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:
1.29 0.298 1.09
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0342
_refine_ls_wR_factor_gt          0.0296
_refine_ls_wR_factor_ref         0.0296
_reflns_limit_h_max              18
_reflns_limit_h_min              -20
_reflns_limit_k_max              16
_reflns_limit_k_min              0
_reflns_limit_l_max              23
_reflns_limit_l_min              0
_reflns_number_gt                5069
_reflns_number_total             7756
_reflns_threshold_expression     I>3.0\s(I)
_oxford_diffrn_Wilson_B_factor   3.09
_oxford_diffrn_Wilson_scale      32.32
_oxford_refine_ls_scale          0.2170(2)
_oxford_structure_analysis_title '9111430 sal0702'
_cod_data_source_file            b916913j.txt
_cod_data_source_block           sal0702
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
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 21/a 1 '
_cod_database_code               7024436