Heterolytic addition of E-H bonds across Pt-P bonds in Pt N-heterocyclic phosphenium/phosphido complexes.
Pan, Baofei; Bezpalko, Mark W.; Foxman, Bruce M.; Thomas, Christine M.; Dalton transactions (Cambridge, England : 2003) 41 (2012) 9083–9090; doi:10.1039/c2dt30455d

data_7019764
_publ_section_title
;
 Heterolytic addition of E-H bonds across Pt-P bonds in Pt N-heterocyclic
 phosphenium/phosphido complexes.
;
_journal_issue                   30
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              9083
_journal_page_last               9090
_journal_paper_doi               10.1039/c2dt30455d
_journal_volume                  41
_journal_year                    2012
_chemical_formula_moiety         'C38 H32 N2 O1 P3 Pt1'
_chemical_formula_sum            'C38 H32 N2 O P3 Pt'
_chemical_formula_weight         820.70
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     other
_audit_creation_date             11-11-11
_audit_creation_method           CRYSTALS_ver_14.30
_cell_angle_alpha                90
_cell_angle_beta                 110.393(1)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   25.0443(7)
_cell_length_b                   15.9342(5)
_cell_length_c                   9.6935(3)
_cell_measurement_reflns_used    9905
_cell_measurement_temperature    120
_cell_measurement_theta_max      29
_cell_measurement_theta_min      2
_cell_volume                     3625.85(19)
_computing_cell_refinement       'Apex2 (Bruker AXS, 2006)'
_computing_data_collection       'Apex2 (Bruker AXS, 2006)'
_computing_data_reduction        'Apex2 (Bruker AXS, 2006)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_diffrn_ambient_temperature      120
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       Area
_diffrn_measurement_device_type  'Bruker Kappa Apex2'
_diffrn_measurement_method       '\f & \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.032
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       -35
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            5303
_diffrn_reflns_theta_full        30.046
_diffrn_reflns_theta_max         30.046
_diffrn_reflns_theta_min         1.545
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.033
_exptl_absorpt_correction_T_max  0.59
_exptl_absorpt_correction_T_min  0.43
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
Analytical Absorption (De Meulenaer & Tompa, 1965)
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.503
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1620
_exptl_crystal_size_max          0.270
_exptl_crystal_size_mid          0.210
_exptl_crystal_size_min          0.130
_platon_squeeze_details
;
During the structure solution, electron density difference
maps revealed that there were considerable disordered
solvent molecules, which could not be successfully modeled.
>From history, the remaining solvate was likely ether or THF
in a volume of 553.9 \%A3 per unit cell (15.3%). It appeared
that the cavity areas contained about four ether and/or THF
molecules, located near the centers of symmetry at (0, 0, 0)
and ( 1/2, 1/2 , 0 ). Modeling with or without restraints
was unsuccessful, as was step by step acquisition
of peaks using successive electron density difference maps.
Thus, the structure factors were modified using the PLATON
SQUEEZE technique, in order to produce a ?solvate-free?
structure factor set. PLATON reported a total electron
density of 174 e- per unit cell, likely representing four THF
or ether molecules, consistent with our earlier observations.
Use of the SQUEEZE technique resulted in a decrease of ca.
1.7 % in R.
;
_refine_diff_density_max         2.01
_refine_diff_density_min         -1.71
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.9968
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     231
_refine_ls_number_reflns         5303
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0348
_refine_ls_R_factor_gt           0.0242
_refine_ls_shift/su_max          0.0014223
_refine_ls_shift/su_mean         0.0000334
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
Method= Modified Sheldrick
w=1/[\s^2^(F^2^) + ( 0.02P)^2^ +12.81P]
,where P=(max(Fo^2^,0) + 2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0605
_refine_ls_wR_factor_gt          0.0550
_refine_ls_wR_factor_ref         0.0605
_reflns_limit_h_max              33
_reflns_limit_h_min              -35
_reflns_limit_k_max              22
_reflns_limit_k_min              0
_reflns_limit_l_max              13
_reflns_limit_l_min              0
_reflns_number_gt                4020
_reflns_number_total             5303
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   0.00
_oxford_diffrn_Wilson_scale      0.00
_oxford_refine_ls_r_factor_ref   0.0348
_oxford_refine_ls_scale          0.046447(4)
_oxford_reflns_number_all        5303
_oxford_reflns_threshold_expression_ref I>0.0\s(I)
_oxford_structure_analysis_title 'bfpan_6169_0m in C2/c'
_cod_data_source_file            c2dt30455d.txt
_cod_data_source_block           7
_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 2.4.1 from
2010-06-29.

'_atom_sites_solution_primary' value 'Other' changed to
'other' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 
;
_cod_original_sg_symbol_H-M      'C 1 2/c 1 '
_cod_original_formula_sum        'C38 H32 N2 O1 P3 Pt1'
_cod_database_code               7019764
_iucr_refine_instruction_details_constraints
;
BLOCK SCALE X'S, U'S
RIDE C ( 2,X'S) H ( 21,X'S)
RIDE C ( 3,X'S) H ( 31,X'S)
RIDE C ( 4,X'S) H ( 41,X'S)
RIDE C ( 5,X'S) H ( 51,X'S)
RIDE C ( 6,X'S) H ( 61,X'S)
RIDE C ( 8,X'S) H ( 81,X'S)
RIDE C ( 9,X'S) H ( 91,X'S)
RIDE C ( 10,X'S) H ( 101,X'S)
RIDE C ( 11,X'S) H ( 111,X'S)
RIDE C ( 12,X'S) H ( 121,X'S)
RIDE C ( 14,X'S) H ( 141,X'S)
RIDE C ( 15,X'S) H ( 151,X'S)
RIDE C ( 16,X'S) H ( 161,X'S)
RIDE C ( 17,X'S) H ( 171,X'S)
RIDE C ( 18,X'S) H ( 181,X'S)
RIDE C ( 19,X'S) H ( 191,X'S) H ( 192,X'S)
RIDE C ( 20,X'S) H ( 201,X'S) H ( 202,X'S)
END
;
_iucr_refine_instruction_details_restraints
;
NO
REM HREST START (DO NOT REMOVE THIS LINE)
REM HREST END (DO NOT REMOVE THIS LINE)
END
;