Transformations between Monomeric, Dimeric, and Trimeric Phosphazanes: Oligomerizing NP Analogues of Olefins
Neil Burford; T. Stanley Cameron; Korey D. Conroy; Bobby Ellis; Michael Lumsden; Charles L. B. Macdonald; Robert McDonald; Andrew D. Phillips; Paul J. Ragogna; Robert W. Schurko; Denise Walsh; Roderick E. Wasylishen; Journal of the American Chemical Society 124 (2002) 14012–14013; doi:10.1021/ja027946o

data_4115335
_publ_contact_author_address
;
Harry Shirreff Professor of Chemical Research 
and Killam Professor
Department of Chemistry
Dalhousie University
Halifax, Nova Scotia B3H 4J3
CANADA
;
_publ_contact_author_email       ' neil.burford@dal.ca '
_publ_contact_author_fax         ' 902-494-1310'
_publ_contact_author_name        ' Neil Burford'
_publ_contact_author_phone       ' 902-494-3190 (lab 3681) '
_publ_section_title
;
 Transformations between Monomeric, Dimeric, and Trimeric Phosphazanes:
 Oligomerizing NP Analogues of Olefins
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              14012
_journal_page_last               14013
_journal_paper_doi               10.1021/ja027946o
_journal_volume                  124
_journal_year                    2002
_chemical_formula_sum            'C19 H29 F3 N O3 P S'
_chemical_formula_weight         439.46
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_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
_cell_angle_alpha                90.00
_cell_angle_beta                 90.56(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.358(2)
_cell_length_b                   16.400(2)
_cell_length_c                   12.006(1)
_cell_measurement_reflns_used    22
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      39.4
_cell_measurement_theta_min      30.4
_cell_volume                     2236.3(5)
_computing_cell_refinement       'MSC/AFC Diffractometer Control'
_computing_data_collection       'MSC/AFC Diffractometer Control'
_computing_data_reduction
'teXsan for Windows version 1.06 (MSC, 1997-1999)'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SIR92 (Altomare, et. al. 1994)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Rigaku AFC5R'
_diffrn_measurement_method       \w-2\q
_diffrn_orient_matrix_UB_11      0.01234
_diffrn_orient_matrix_UB_12      0.03604
_diffrn_orient_matrix_UB_13      0.06630
_diffrn_orient_matrix_UB_21      -0.00512
_diffrn_orient_matrix_UB_22      -0.04854
_diffrn_orient_matrix_UB_23      0.05011
_diffrn_orient_matrix_UB_31      0.08703
_diffrn_orient_matrix_UB_32      -0.00796
_diffrn_orient_matrix_UB_33      -0.00563
_diffrn_radiation_detector       'scintillation counter'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Rigaku rotating anode'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0589
_diffrn_reflns_av_sigmaI/netI    0.2273
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            3985
_diffrn_reflns_reduction_process 'Lp corrections applied'
_diffrn_reflns_theta_max         63.68
_diffrn_reflns_theta_min         2.69
_diffrn_standards_decay_%        0.69
_diffrn_standards_interval_count 150
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    2.353
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.758
_exptl_absorpt_correction_type
;
\y scans (North,Phillips & Matthews, 1968)
;
_exptl_crystal_colour            'light yellow'
_exptl_crystal_density_diffrn    1.305
_exptl_crystal_description       block
_exptl_crystal_F_000             928
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.317
_refine_diff_density_min         -0.305
_refine_diff_density_rms         0.071
_refine_ls_extinction_coef       0.0006(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_all   1.037
_refine_ls_goodness_of_fit_obs   1.298
_refine_ls_matrix_type           full
_refine_ls_number_parameters     200
_refine_ls_number_reflns         3628
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.037
_refine_ls_restrained_S_obs      1.298
_refine_ls_R_factor_all          0.2624
_refine_ls_R_factor_obs          0.0579
_refine_ls_shift/esd_max         -0.028
_refine_ls_shift/esd_mean        0.006
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'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_all         0.2420
_refine_ls_wR_factor_obs         0.1596
_reflns_number_observed          1108
_reflns_number_total             3628
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ja027946o_s1_2.cif
_cod_data_source_block           wlsh21twin_Compound2b[Mes*NPOTf]2
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        2236.1(4)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_original_formula_sum        'C19 H29 F3 N1 O3 P1 S'
_cod_database_code               4115335