Adaptable ligand donor strength: tracking transannular bond interactions in tris(2-pyridylmethyl)-azaphosphatrane (TPAP).
Thammavongsy, Zachary; Cunningham, Drew W.; Sutthirat, Natwara; Eisenhart, Reed J.; Ziller, Joseph W.; Yang, Jenny Y.; Dalton transactions (Cambridge, England : 2003) 47 (2018) 14101–14110; doi:10.1039/c8dt03180k

data_7047548
_publ_section_title
;
 Adaptable ligand donor strength: tracking transannular bond interactions
 in tris(2-pyridylmethyl)-azaphosphatrane (TPAP).
;
_journal_issue                   39
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              14101
_journal_page_last               14110
_journal_paper_doi               10.1039/c8dt03180k
_journal_volume                  47
_journal_year                    2018
_chemical_formula_sum            'C28 H36 B2 F8 N9 Ni P'
_chemical_formula_weight         761.96
_chemical_name_common            '[NiTPAP(CH3CN)][BF4]2'
_chemical_name_systematic        '[NiTPAP(CH3CN)][BF4]2'
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2018-03-02 deposited with the CCDC.
2018-09-14 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 98.9026(17)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.0563(17)
_cell_length_b                   20.118(4)
_cell_length_c                   18.435(4)
_cell_measurement_reflns_used    9904
_cell_measurement_temperature    88(2)
_cell_measurement_theta_max      28.88
_cell_measurement_theta_min      2.24
_cell_volume                     3318.3(12)
_computing_cell_refinement       'Bruker SAINT 8.34a, 2013'
_computing_data_collection       'Bruker APEX2 2014.1-1, 2014'
_computing_data_reduction        'Bruker SAINT 8.34a, 2013'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'Bruker SHELXTL 2014/4'
_diffrn_ambient_temperature      88(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.951
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0386
_diffrn_reflns_av_unetI/netI     0.0331
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.951
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            40781
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.951
_diffrn_reflns_theta_full        25.500
_diffrn_reflns_theta_max         29.077
_diffrn_reflns_theta_min         2.025
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.714
_exptl_absorpt_correction_T_max  0.7458
_exptl_absorpt_correction_T_min  0.6681
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker SADABS 2014/5'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.525
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    not_measured
_exptl_crystal_description       Irregular
_exptl_crystal_F_000             1568
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Acetonitrile / Diethyl Ether'
_exptl_crystal_size_max          0.437
_exptl_crystal_size_mid          0.238
_exptl_crystal_size_min          0.178
_refine_diff_density_max         1.173
_refine_diff_density_min         -0.945
_refine_diff_density_rms         0.077
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     462
_refine_ls_number_reflns         8456
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.0583
_refine_ls_R_factor_gt           0.0454
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0570P)^2^+4.5044P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1187
_refine_ls_wR_factor_ref         0.1267
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6941
_reflns_number_total             8456
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt03180k2.cif
_cod_data_source_block           jyy156
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not_measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 4973 2017-02-22 13:04:09Z antanas 

 Adding full bibliography for 7047545--7047550.cif.
;
_cod_original_cell_volume        3318.3(11)
_cod_database_code               7047548
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.745
_shelx_estimated_absorpt_t_max   0.883
_exptl_absorpt_special_details
; 
 Reflections not merged 
   82592 Corrected reflections written to file jyy156s.hkl 
 Estimated minimum and maximum transmission:  0.6681  0.7458 
 The ratio (0.8958) of these values is more reliable than their absolute values! 
 Additional spherical absorption correction applied with mu*r =  0.2000 
 Lambda/2 correction factor = 0.00150 
;
_shelx_res_checksum              55613