Pseudoheptacoordination and Pseudohexacoordination in Tris(2-N,N-dimethylbenzylamino)phosphane
A. Chandrasekaran; Natalya V. Timosheva; Roberta O. Day; Robert R. Holmes; Inorganic Chemistry 41 (2002) 5235–5240; doi:10.1021/ic020153i

data_4318545
_publ_section_title
;
 Pseudoheptacoordination and Pseudohexacoordination in
 Tris(2-N,N-dimethylbenzylamino)phosphane
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5235
_journal_page_last               5240
_journal_paper_doi               10.1021/ic020153i
_journal_volume                  41
_journal_year                    2002
_chemical_formula_sum            'C27 H47 N3 O13.5 P'
_chemical_formula_weight         660.65
_chemical_name_systematic
; 
 ? 
;
_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
_cell_angle_alpha                90.00
_cell_angle_beta                 113.3568(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.14430(10)
_cell_length_b                   25.4053(4)
_cell_length_c                   12.7431(2)
_cell_measurement_temperature    293(2)
_cell_volume                     3312.23(8)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.974
_diffrn_measured_fraction_theta_max 0.974
_diffrn_measurement_device_type  'Nonius KappaCCD area detector'
_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  0.0188
_diffrn_reflns_av_sigmaI/netI    0.0343
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            10658
_diffrn_reflns_theta_full        25.02
_diffrn_reflns_theta_max         25.02
_diffrn_reflns_theta_min         4.23
_exptl_absorpt_coefficient_mu    0.151
_exptl_absorpt_correction_T_max  0.9562
_exptl_absorpt_correction_T_min  0.8954
_exptl_crystal_density_diffrn    1.325
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1412
_exptl_crystal_size_max          0.75
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.30
_refine_diff_density_max         0.772
_refine_diff_density_min         -0.704
_refine_diff_density_rms         0.085
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.077
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     360
_refine_ls_number_reflns         5693
_refine_ls_number_restraints     10
_refine_ls_restrained_S_all      1.086
_refine_ls_R_factor_all          0.1236
_refine_ls_R_factor_gt           0.1042
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1773P)^2^+5.1747P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2945
_refine_ls_wR_factor_ref         0.3145
_reflns_number_gt                4394
_reflns_number_total             5693
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic020153i_s1_3.cif
_cod_data_source_block           ntp1a
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_original_formula_sum        'C27 H47 N3 O13.50 P'
_cod_database_code               4318545