N-Heterocyclic Phosphenium Ligands as Sterically and Electronically-Tunable Isolobal Analogues of Nitrosyls
Baofei Pan; Zhequan Xu; Mark W. Bezpalko; Bruce M. Foxman; Christine M. Thomas; Inorganic Chemistry 51 (2012) 4170–4179; doi:10.1021/ic202581v

data_4328801
_publ_section_title
;
 N-Heterocyclic Phosphenium Ligands as Sterically and
 Electronically-Tunable Isolobal Analogues of Nitrosyls
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4170
_journal_page_last               4179
_journal_paper_doi               10.1021/ic202581v
_journal_volume                  51
_journal_year                    2012
_chemical_formula_moiety         'C38 H32 I1.50 N2 P3 Pt1.50'
_chemical_formula_sum            'C38 H32 I1.5 N2 P3 Pt1.5'
_chemical_formula_weight         1092.60
_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             11-05-15
_audit_creation_method           CRYSTALS_ver_14.21
_cell_angle_alpha                90
_cell_angle_beta                 95.387(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   18.6542(8)
_cell_length_b                   19.9824(8)
_cell_length_c                   22.1057(10)
_cell_measurement_reflns_used    9949
_cell_measurement_temperature    120
_cell_measurement_theta_max      28
_cell_measurement_theta_min      3
_cell_volume                     8203.6(6)
_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    'Superflip (Palatinus & Chapuis, 2007)'
_diffrn_ambient_temperature      120
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_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       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            9888
_diffrn_reflns_theta_full        28.027
_diffrn_reflns_theta_max         28.027
_diffrn_reflns_theta_min         1.705
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    6.389
_exptl_absorpt_correction_T_max  0.25
_exptl_absorpt_correction_T_min  0.20
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
; 
 Analytical Absorption (De Meulenaer & Tompa, 1965) 
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.769
_exptl_crystal_description       prism
_exptl_crystal_F_000             4124
_exptl_crystal_size_max          0.561
_exptl_crystal_size_mid          0.255
_exptl_crystal_size_min          0.216
_platon_squeeze_details
;
During the structure solutions, electron density difference 
maps revealed that there were considerable disordered solvent 
molecules.  From history, the solvate was likely Et2O, THF or 
both in a volume of 1698.5 \%A3 per unit cell 
(20.7 %); the peaks, represented a nearly continuous 
chain of electron density through channels in the unit cell, 
and could not be modeled successfully.  It appeared that the 
cavity areas contained about eight diethyl ether or THF molecules. 
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 370 e- per unit cell, 
likely representing eight diethyl ether or THF molecules, 
consistent with our earlier observations.  Use of the 
SQUEEZE technique resulted in a decrease of ca 0.5% in R.
;
_refine_diff_density_max         3.89
_refine_diff_density_min         -1.96
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.0181
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     416
_refine_ls_number_reflns         9888
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0452
_refine_ls_R_factor_gt           0.0321
_refine_ls_shift/su_max          0.0027241
_refine_ls_shift/su_mean         0.0000405
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method= Modified Sheldrick 
 w=1/[\s^2^(F^2^) + ( 0.03P)^2^ +*****P] 
 ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0831
_refine_ls_wR_factor_gt          0.0756
_refine_ls_wR_factor_ref         0.0831
_reflns_limit_h_max              24
_reflns_limit_h_min              -24
_reflns_limit_k_max              26
_reflns_limit_k_min              0
_reflns_limit_l_max              29
_reflns_limit_l_min              0
_reflns_number_gt                7916
_reflns_number_total             9888
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   1.66
_oxford_diffrn_Wilson_scale      1138.27
_oxford_refine_ls_r_factor_ref   0.0452
_oxford_refine_ls_scale          0.0213166(8)
_oxford_reflns_number_all        9888
_oxford_reflns_threshold_expression_ref I>-10.0\s(I)
_oxford_structure_analysis_title 'bfpan_170_0m in C2/c'
_cod_data_source_file            ic202581v_si_002_09.cif
_cod_data_source_block           14
_cod_depositor_comments
;
The following automatic conversions were performed:

'_atom_sites_solution_primary' value 'Other' changed to 'other'
according to the built-in table from CIF Core 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 I1.50 N2 P3 Pt1.50'
_cod_database_code               4328801
_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   (  19,X'S) H   ( 191,X'S) H   ( 192,X'S) 
RIDE C   (  20,X'S) H   ( 201,X'S) H   ( 202,X'S) 
RIDE C   (  22,X'S) H   ( 221,X'S) 
RIDE C   (  23,X'S) H   ( 231,X'S) 
RIDE C   (  24,X'S) H   ( 241,X'S) 
RIDE C   (  25,X'S) H   ( 251,X'S) 
RIDE C   (  28,X'S) H   ( 281,X'S) 
RIDE C   (  29,X'S) H   ( 291,X'S) 
RIDE C   (  30,X'S) H   ( 301,X'S) 
RIDE C   (  31,X'S) H   ( 311,X'S) 
RIDE C   (  32,X'S) H   ( 321,X'S) 
RIDE C   (  34,X'S) H   ( 341,X'S) 
RIDE C   (  35,X'S) H   ( 351,X'S) 
RIDE C   (  36,X'S) H   ( 361,X'S) 
RIDE C   (  37,X'S) H   ( 371,X'S) 
RIDE C   (  38,X'S) H   ( 381,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                                                                             
;