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_7047549
_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_moiety         'C24 H30 Cl Co N7 P'
_chemical_formula_sum            'C24 H30 Cl Co N7 P'
_chemical_formula_weight         541.90
_chemical_name_systematic        Co(TPAP)Cl
_chemical_properties_physical    Air-sensitive
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2018-05-04 deposited with the CCDC.
2018-09-14 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 100.490(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.8827(5)
_cell_length_b                   14.0100(7)
_cell_length_c                   17.8800(9)
_cell_measurement_reflns_used    9913
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      68.43
_cell_measurement_theta_min      3.15
_cell_volume                     2434.2(2)
_computing_cell_refinement       'SAINT, Bruker'
_computing_data_collection       'APEX II, Bruker'
_computing_data_reduction        'SAINT, Bruker'
_computing_molecular_graphics    'SHELXTL, Bruker'
_computing_publication_material  'SHELXTL, Bruker'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      123(2)
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_device_type  'Bruker D8 Photon 100 CMOS'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0486
_diffrn_reflns_av_unetI/netI     0.0436
_diffrn_reflns_Laue_measured_fraction_full 0.985
_diffrn_reflns_Laue_measured_fraction_max 0.983
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            17925
_diffrn_reflns_point_group_measured_fraction_full 0.985
_diffrn_reflns_point_group_measured_fraction_max 0.983
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         68.429
_diffrn_reflns_theta_min         4.035
_diffrn_source                   'micro-focus sealed tube'
_exptl_absorpt_coefficient_mu    7.379
_exptl_absorpt_correction_T_max  0.7531
_exptl_absorpt_correction_T_min  0.3350
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, R. Blessing, 1995'
_exptl_crystal_colour            Purple
_exptl_crystal_density_diffrn    1.479
_exptl_crystal_description       Block
_exptl_crystal_F_000             1128
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: THF/Pentane'
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.200
_exptl_transmission_factor_max   0.7531
_exptl_transmission_factor_min   0.3350
_refine_diff_density_max         0.561
_refine_diff_density_min         -0.856
_refine_diff_density_rms         0.073
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     307
_refine_ls_number_reflns         4398
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0445
_refine_ls_R_factor_gt           0.0420
_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^)+(0.0516P)^2^+3.4268P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1070
_refine_ls_wR_factor_ref         0.1092
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4161
_reflns_number_total             4398
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt03180k2.cif
_cod_data_source_block           15073z
_cod_depositor_comments
'Adding full bibliography for 7047545--7047550.cif.'
_cod_database_code               7047549
_shelx_estimated_absorpt_t_min   0.320
_shelx_estimated_absorpt_t_max   0.320
_shelx_res_checksum              48010