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_4328795
_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         'C30 H27.50 F3 N1 O0.50 P2.50 Pt0.50'
_chemical_formula_sum            'C30 H27.5 F3 N O0.5 P2.5 Pt0.5'
_chemical_formula_weight         642.03
_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     other
_audit_creation_date             11-03-06
_audit_creation_method           CRYSTALS_ver_14.15
_cell_angle_alpha                90.4310(10)
_cell_angle_beta                 95.7350(10)
_cell_angle_gamma                106.0290(10)
_cell_formula_units_Z            4
_cell_length_a                   11.3985(3)
_cell_length_b                   13.0341(3)
_cell_length_c                   19.9056(5)
_cell_measurement_reflns_used    9961
_cell_measurement_temperature    120
_cell_measurement_theta_max      28
_cell_measurement_theta_min      2
_cell_volume                     2826.25(12)
_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 0.999
_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  0.045
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            13634
_diffrn_reflns_theta_full        28.001
_diffrn_reflns_theta_max         28.001
_diffrn_reflns_theta_min         1.869
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.686
_exptl_absorpt_correction_T_max  0.85
_exptl_absorpt_correction_T_min  0.50
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
; 
 Analytical Absorption (De Meulenaer & Tompa, 1965) 
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.509
_exptl_crystal_description       'plate fragment'
_exptl_crystal_F_000             1288
_exptl_crystal_size_max          0.356
_exptl_crystal_size_mid          0.260
_exptl_crystal_size_min          0.060
_platon_squeeze_details
;
During the structure solution, electron density difference 
maps revealed that there were considerable disordered 
solvent molecules.  One THF molecule was located and 
successfully refined.  From history, the remaining solvate 
was likely THF, ether or pentane in a volume of 306.4 \%A3 
per unit cell (10.8%); the remaining peaks could not be 
modeled successfully.  It appeared that the cavity area 
contained about two THF molecules, located near the 
center of symmetry at  (0, 1/2, 1/2 ).  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 
(only for the second independent THF molecule.  PLATON 
reported a total electron density of 72 e- per unit cell, 
likely representing two THF molecules, consistent with 
our earlier observations.  Use of the SQUEEZE technique 
resulted in a decrease of ca 1.8 % in R.  
;
_refine_diff_density_max         1.18
_refine_diff_density_min         -1.02
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.9667
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     679
_refine_ls_number_reflns         13634
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0340
_refine_ls_R_factor_gt           0.0269
_refine_ls_shift/su_max          0.0030408
_refine_ls_shift/su_mean         0.0000732
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method= Modified Sheldrick 
 w=1/[\s^2^(F^2^) + ( 0.02P)^2^ + 2.63P] 
 ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0573
_refine_ls_wR_factor_gt          0.0558
_refine_ls_wR_factor_ref         0.0573
_reflns_limit_h_max              14
_reflns_limit_h_min              -15
_reflns_limit_k_max              17
_reflns_limit_k_min              -17
_reflns_limit_l_max              26
_reflns_limit_l_min              0
_reflns_number_gt                11929
_reflns_number_total             13634
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   1.06
_oxford_diffrn_Wilson_scale      377.69
_oxford_refine_ls_r_factor_ref   0.0340
_oxford_refine_ls_scale          0.103818(11)
_oxford_reflns_number_all        13634
_oxford_reflns_threshold_expression_ref I>-10.0\s(I)
_oxford_structure_analysis_title 'bfpan_123_0m in P-1'
_cod_data_source_file            ic202581v_si_002_03.cif
_cod_data_source_block           3
_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      'P -1 '
_cod_original_formula_sum        'C30 H27.50 F3 N1 O0.50 P2.50 Pt0.50'
_cod_database_code               4328795
_iucr_refine_instruction_details_constraints
;
BLOCK SCALE X'S, U'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                                                                             
;