Electronic and steric Tolman parameters for proazaphosphatranes, the superbase core of the tri(pyridylmethyl)azaphosphatrane (TPAP) ligand.
Thammavongsy, Zachary; Kha, Ivy M.; Ziller, Joseph W.; Yang, Jenny Y.; Dalton transactions (Cambridge, England : 2003) 45 (2016) 9853–9859; doi:10.1039/c6dt00326e

data_7038545
_publ_section_title
;
 Electronic and steric Tolman parameters for proazaphosphatranes, the
 superbase core of the tri(pyridylmethyl)azaphosphatrane (TPAP) ligand.
;
_journal_issue                   24
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              9853
_journal_page_last               9859
_journal_paper_doi               10.1039/c6dt00326e
_journal_volume                  45
_journal_year                    2016
_chemical_formula_sum            'C21 H39 N4 Ni O3 P'
_chemical_formula_weight         485.24
_chemical_name_common            Ni(LiBu)(CO)3
_chemical_name_systematic
'[Nickle(0)-tricarbonyl-(2,8,9-triisobutyl-2,3,8,9-tetraaza-1-phosphabicyclo[3,3,3]undecane)]'
_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   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2016-01-19 deposited with the CCDC.
2016-02-16 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 97.2348(6)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.4524(5)
_cell_length_b                   17.9047(8)
_cell_length_c                   13.5993(6)
_cell_measurement_reflns_used    9976
_cell_measurement_temperature    88(2)
_cell_measurement_theta_max      28.96
_cell_measurement_theta_min      2.27
_cell_volume                     2524.8(2)
_computing_cell_refinement       'Bruker SAINT 8.34a, 2013'
_computing_data_collection       'Bruker APEX2 2014.11-0, 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 0.999
_diffrn_measured_fraction_theta_max 0.946
_diffrn_measurement_device_type  'Bruker SMART 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  0.0258
_diffrn_reflns_av_unetI/netI     0.0219
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.946
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            31264
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.946
_diffrn_reflns_theta_full        25.500
_diffrn_reflns_theta_max         29.204
_diffrn_reflns_theta_min         1.890
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.859
_exptl_absorpt_correction_T_max  0.9423
_exptl_absorpt_correction_T_min  0.8177
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'Bruker SADABS 2014/5'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.277
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    not_measured
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1040
_exptl_crystal_size_max          0.287
_exptl_crystal_size_mid          0.235
_exptl_crystal_size_min          0.139
_refine_diff_density_max         0.581
_refine_diff_density_min         -0.234
_refine_diff_density_rms         0.051
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     431
_refine_ls_number_reflns         6479
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.0341
_refine_ls_R_factor_gt           0.0272
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0363P)^2^+0.8703P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0665
_refine_ls_wR_factor_ref         0.0701
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5607
_reflns_number_total             6479
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt00326e2.cif
_cod_data_source_block           jyy72
_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 4268 2015-11-12 08:31:59Z antanas 

 Adding full bibliography for 7038544--7038548.cif.
;
_cod_database_code               7038545
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.791
_shelx_estimated_absorpt_t_max   0.890
_shelx_res_checksum              25802