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_7038546
_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            'C30 H33 N4 Ni O3 P'
_chemical_formula_weight         587.28
_chemical_name_common            Ni(LBz)(CO)3
_chemical_name_systematic
'[Nickle(0)-tricarbonyl-(2,8,9-tribenzyl-2,3,8,9-tetraaza-1-phosphabicyclo[3,3,3]undecane)]'
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2016-01-19 deposited with the CCDC.
2016-02-16 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 99.3160(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.7263(8)
_cell_length_b                   23.412(2)
_cell_length_c                   12.5881(11)
_cell_measurement_reflns_used    9924
_cell_measurement_temperature    133(2)
_cell_measurement_theta_max      29.00
_cell_measurement_theta_min      2.29
_cell_volume                     2828.7(4)
_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-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      133(2)
_diffrn_measured_fraction_theta_full 1.000
_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_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0433
_diffrn_reflns_av_sigmaI/netI    0.0214
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            70276
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         29.23
_diffrn_reflns_theta_min         1.74
_exptl_absorpt_coefficient_mu    0.781
_exptl_absorpt_correction_T_max  0.8748
_exptl_absorpt_correction_T_min  0.7788
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'Bruker SADABS 2014/5'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.379
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1232
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.18
_refine_diff_density_max         1.370
_refine_diff_density_min         -0.630
_refine_diff_density_rms         0.084
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.168
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     352
_refine_ls_number_reflns         7270
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.168
_refine_ls_R_factor_all          0.0470
_refine_ls_R_factor_gt           0.0400
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1283
_refine_ls_wR_factor_ref         0.1393
_reflns_number_gt                6422
_reflns_number_total             7270
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c6dt00326e2.cif
_cod_data_source_block           jyy74s
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to
/usr/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

'_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_original_cell_volume        2828.6(4)
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               7038546