Chalcogeno-urea Ligands on a Phosphadiazonium Lewis Acceptor: A New Synthetic Approach to Ch-P Bonds (Ch = O, S, Se)
Neil Burford; Andrew D. Phillips; Heather A. Spinney; Katherine N. Robertson; T. Stanley Cameron; Robert McDonald; Inorganic Chemistry 42 (2003) 4949–4954; doi:10.1021/ic034182k

data_4313947
_publ_contact_author_address
;
Department of Chemistry
Dalhousie University
Halifax, Nova Scotia
B3H 4J3
;
_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 '
_publ_section_title
;
 Chalcogeno-urea Ligands on a Phosphadiazonium Lewis Acceptor: A New
 Synthetic Approach to Ch-P Bonds (Ch = O, S, Se)
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4949
_journal_page_last               4954
_journal_paper_doi               10.1021/ic034182k
_journal_volume                  42
_journal_year                    2003
_chemical_formula_sum            'C5.5 H10 N S0.5'
_chemical_formula_weight         106.18
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      15
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 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
_cell_angle_beta                 102.63(5)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   10.024(7)
_cell_length_b                   11.298(7)
_cell_length_c                   11.358(7)
_cell_measurement_reflns_used    22
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      15.8
_cell_measurement_theta_min      10.0
_cell_volume                     1255.2(14)
_computing_cell_refinement       'MSC/AFC Diffractometer Control'
_computing_data_collection       'MSC/AFC Diffractometer Control'
_computing_data_reduction
;
teXsan for Windows version 1.05 (MSC, 1997-1999) 
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR-92 (Altomare et al., 1994) '
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.355
_diffrn_measured_fraction_theta_max 0.355
_diffrn_measurement_device_type  'Rigaku AFC5R'
_diffrn_measurement_method       \w-2\q
_diffrn_orient_matrix_UB_11      -0.07472
_diffrn_orient_matrix_UB_12      0.06040
_diffrn_orient_matrix_UB_13      -0.01316
_diffrn_orient_matrix_UB_21      0.06970
_diffrn_orient_matrix_UB_22      0.06469
_diffrn_orient_matrix_UB_23      0.01056
_diffrn_orient_matrix_UB_31      -0.00336
_diffrn_orient_matrix_UB_32      -0.00126
_diffrn_orient_matrix_UB_33      -0.08863
_diffrn_radiation_detector       'scintillation counter'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Rigaku rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0983
_diffrn_reflns_av_sigmaI/netI    0.167
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            1535
_diffrn_reflns_reduction_process 'Lp corrections applied'
_diffrn_reflns_theta_full        30.07
_diffrn_reflns_theta_max         30.07
_diffrn_reflns_theta_min         2.76
_diffrn_standards_decay_%        -3.94
_diffrn_standards_interval_count 150
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.226
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.784
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details   'North,Phillips & Matthews (1968)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.124
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'long thin rod'
_exptl_crystal_F_000             464
_exptl_crystal_size_max          0.90
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.177
_refine_diff_density_min         -0.147
_refine_diff_density_rms         0.039
_refine_ls_extinction_coef       0.0022(17)
_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   0.936
_refine_ls_hydrogen_treatment    'riding model'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     84
_refine_ls_number_reflns         1370
_refine_ls_number_restraints     33
_refine_ls_restrained_S_all      0.932
_refine_ls_R_factor_all          0.2557
_refine_ls_R_factor_obs          0.0433
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0738P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1833
_refine_ls_wR_factor_obs         0.1168
_reflns_number_gt                382
_reflns_number_total             1370
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic034182ksi20030218_083705_2.cif
_cod_data_source_block           SIm
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0738P)^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^)+(0.0738P)^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        1255(1)
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_original_formula_sum        'C5.50 H10 N1 S0.50'
_cod_database_code               4313947