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_4344095
_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_absolute_configuration ad
_chemical_formula_moiety         'C89 H79 B1 N2 Ni1 P4'
_chemical_formula_sum            'C89 H79 B N2 Ni P4'
_chemical_formula_weight         1370.04
_space_group_IT_number           1
_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             2015-05-13
_audit_creation_method           CRYSTALS_ver_14.61
_cell_angle_alpha                102.169(3)
_cell_angle_beta                 101.766(2)
_cell_angle_gamma                100.942(2)
_cell_formula_units_Z            2
_cell_length_a                   12.0649(6)
_cell_length_b                   15.9904(8)
_cell_length_c                   21.2462(11)
_cell_measurement_reflns_used    9945
_cell_measurement_temperature    120
_cell_measurement_theta_max      30
_cell_measurement_theta_min      3
_cell_volume                     3804.8(3)
_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 0.998
_diffrn_measured_fraction_theta_max 0.991
_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  0.000
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            45004
_diffrn_reflns_theta_full        29.708
_diffrn_reflns_theta_max         30.315
_diffrn_reflns_theta_min         1.778
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.385
_exptl_absorpt_correction_T_max  0.88
_exptl_absorpt_correction_T_min  0.88
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
; 
 Analytical Absorption (De Meulenaer & Tompa, 1965) 
;
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.196
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       priam
_exptl_crystal_F_000             1440
_exptl_crystal_size_max          0.520
_exptl_crystal_size_mid          0.340
_exptl_crystal_size_min          0.320
_platon_squeeze_details
;
During the structure solution, electron density difference 
maps revealed that there was considerable disorder, associated 
with ether solvent molecule(s), which could not be successfully 
modeled.  From history, the remaining solvate was likely ether 
in a volume of 374.9 \%A3 per unit cell (9.9%).  It appeared that 
the cavity area contained about two ether molecules, located near 
the location (-0.156, 0.229, 0.429), as shown in the bc projection.
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 
96 e- per unit cell, likely representing about two ether molecules, 
consistent with our earlier observations.  Use of the SQUEEZE 
technique resulted in a decrease of ca. 1.6 % in R.  
;
_refine_diff_density_max         1.00
_refine_diff_density_min         -0.62
_refine_ls_abs_structure_details 'Flack (1983), 22887 Friedel-pairs'
_refine_ls_abs_structure_Flack   0.376(6)
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.9888
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1748
_refine_ls_number_reflns         45004
_refine_ls_number_restraints     3
_refine_ls_R_factor_all          0.0730
_refine_ls_R_factor_gt           0.0583
_refine_ls_shift/su_max          0.0020837
_refine_ls_shift/su_mean         0.0003171
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method= Modified Sheldrick 
 w=1/[\s^2^(F^2^) + ( 0.09P)^2^ + 1.87P] 
 ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1526
_refine_ls_wR_factor_gt          0.1435
_refine_ls_wR_factor_ref         0.1526
_reflns_limit_h_max              17
_reflns_limit_h_min              -17
_reflns_limit_k_max              22
_reflns_limit_k_min              -22
_reflns_limit_l_max              30
_reflns_limit_l_min              -30
_reflns_number_gt                37783
_reflns_number_total             45004
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   1.59
_oxford_diffrn_Wilson_scale      116.89
_oxford_refine_ls_r_factor_ref   0.0730
_oxford_refine_ls_scale          2.875(13)
_oxford_reflns_number_all        45004
_oxford_reflns_threshold_expression_ref I>-10.0\s(I)
_oxford_structure_analysis_title 'mwb5_017_0m in P1'
_cod_data_source_file            ic5b01363_si_002.cif
_cod_data_source_block           7
_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_sg_symbol_Hall     'P 1 '
_cod_original_sg_symbol_H-M      'P 1 '
_cod_original_formula_sum        'C89 H79 B1 N2 Ni1 P4'
_cod_database_code               4344095
_platon_squeeze_void_probe_radius 1.20