Use of a Bidentate Ligand Featuring an N-Heterocyclic Phosphenium Cation (NHP(+)) to Systematically Explore the Bonding of NHP(+) Ligands with Nickel.
Bezpalko, Mark W.; Foxman, Bruce M.; Thomas, Christine M.; Inorganic chemistry 54 (2015) 8717–8726; doi:10.1021/acs.inorgchem.5b01363

data_4344096
_publ_section_title
;
 Use of a Bidentate Ligand Featuring an N-Heterocyclic Phosphenium Cation
 (NHP(+)) to Systematically Explore the Bonding of NHP(+) Ligands with
 Nickel.
;
_journal_issue                   17
_journal_name_full               'Inorganic chemistry'
_journal_page_first              8717
_journal_page_last               8726
_journal_paper_doi               10.1021/acs.inorgchem.5b01363
_journal_volume                  54
_journal_year                    2015
_chemical_formula_moiety         'C29 H29 Cl3 N2 Ni1 P2'
_chemical_formula_sum            'C29 H29 Cl3 N2 Ni P2'
_chemical_formula_weight         632.58
_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   difmap
_atom_sites_solution_primary     other
_audit_creation_date             2015-02-19
_audit_creation_method           CRYSTALS_ver_14.61
_cell_angle_alpha                93.425(3)
_cell_angle_beta                 95.166(3)
_cell_angle_gamma                114.410(2)
_cell_formula_units_Z            2
_cell_length_a                   9.8400(5)
_cell_length_b                   10.0200(6)
_cell_length_c                   16.7632(9)
_cell_measurement_reflns_used    8250
_cell_measurement_temperature    120
_cell_measurement_theta_max      30
_cell_measurement_theta_min      2
_cell_volume                     1490.35(14)
_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 0.995
_diffrn_measured_fraction_theta_max 0.995
_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  0.047
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            8657
_diffrn_reflns_theta_full        30.016
_diffrn_reflns_theta_max         30.016
_diffrn_reflns_theta_min         2.245
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.049
_exptl_absorpt_correction_T_max  0.92
_exptl_absorpt_correction_T_min  0.79
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
; 
 Analytical Absorption (De Meulenaer & Tompa, 1965) 
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.410
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             652
_exptl_crystal_size_max          0.220
_exptl_crystal_size_mid          0.210
_exptl_crystal_size_min          0.080
_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 DCM in a volume 
of 111.7 \%A3 per unit cell (7.5%).  It appeared that the 
cavity area contained about one DCM molecule, located near 
a center of symmetry at (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 40 e- per unit cell, likely 
representing one DCM molecule, consistent with our earlier 
observations.  Use of the SQUEEZE technique resulted in a 
decrease of ca. 10.9 % in R.  
;
_refine_diff_density_max         0.68
_refine_diff_density_min         -0.60
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.0000
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     334
_refine_ls_number_reflns         8657
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0489
_refine_ls_R_factor_gt           0.0336
_refine_ls_shift/su_max          0.0004855
_refine_ls_shift/su_mean         0.0000249
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method= Modified Sheldrick 
 w=1/[\s^2^(F^2^) + ( 0.04P)^2^ + 0.83P] 
 ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0792
_refine_ls_wR_factor_gt          0.0742
_refine_ls_wR_factor_ref         0.0792
_reflns_limit_h_max              13
_reflns_limit_h_min              -13
_reflns_limit_k_max              14
_reflns_limit_k_min              -14
_reflns_limit_l_max              23
_reflns_limit_l_min              0
_reflns_number_gt                6641
_reflns_number_total             8657
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   1.35
_oxford_diffrn_Wilson_scale      27.61
_oxford_refine_ls_r_factor_ref   0.0489
_oxford_refine_ls_scale          0.18573(6)
_oxford_reflns_number_all        8657
_oxford_reflns_threshold_expression_ref I>-10.0\s(I)
_oxford_structure_analysis_title 'mwb4_153_0m in P-1'
_cod_data_source_file            ic5b01363_si_002.cif
_cod_data_source_block           8
_cod_depositor_comments
;
The following automatic conversions were performed:

'_atom_sites_solution_primary' value 'Other' changed to 'other'
according to
/usr/data/users/saulius/crontab/automatic-downloads/rss-feeds/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 3271 2015-04-21 07:52:19Z andrius 

 Adding full bibliography for 4344091--4344096.cif.
;
_cod_original_cell_volume        1490.36(8)
_cod_original_sg_symbol_Hall     '-P 1 '
_cod_original_sg_symbol_H-M      'P -1 '
_cod_original_formula_sum        'C29 H29 Cl3 N2 Ni1 P2'
_cod_database_code               4344096