Syntheses and Structures of Heterobicyclic Bis(tert-butylamido)cyclodiphosph(III)azane Compounds Having Phosphorus(III) and Arsenic(III) Centers
Ingo Schranz; Luke P. Grocholl; Lothar Stahl; Richard J. Staples; Alison Johnson; Inorganic Chemistry 39 (2000) 3037–3041; doi:10.1021/ic991405r

data_4321129
_publ_section_title
;
 Syntheses and Structures of Heterobicyclic
 Bis(tert-butylamido)cyclodiphosph(III)azane Compounds Having
 Phosphorus(III) and Arsenic(III) Centers
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3037
_journal_page_last               3041
_journal_paper_doi               10.1021/ic991405r
_journal_volume                  39
_journal_year                    2000
_chemical_formula_sum            'C16 H34 As Cl N4 P2'
_chemical_formula_weight         454.78
_space_group_IT_number           11
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yb'
_symmetry_space_group_name_H-M   'P 1 21/m 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                 97.80(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   9.688(3)
_cell_length_b                   11.873(3)
_cell_length_c                   9.975(3)
_cell_measurement_reflns_used    58
_cell_measurement_temperature    213(2)
_cell_measurement_theta_max      20.81
_cell_measurement_theta_min      3.24
_cell_volume                     1136.8(6)
_computing_cell_refinement       'SMART (SIEMENS, V4.033, 1994)'
_computing_data_collection       'ASTRO (SIEMENS, V4.033, 1994)'
_computing_data_reduction        'SAINT (SIEMENS, V4.035, 1994)'
_computing_molecular_graphics    'SHELXTL (SIEMENS, 1994, ver 5.04)'
_computing_publication_material  'CIFTAB (Sheldrick, 1993)'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      213(2)
_diffrn_measurement_device       'Siemens CCD'
_diffrn_measurement_method       '\w, 0.3 deg'
_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  0.0232
_diffrn_reflns_av_sigmaI/netI    0.0322
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            6978
_diffrn_reflns_theta_max         28.30
_diffrn_reflns_theta_min         2.06
_diffrn_standards_decay_%        <1
_diffrn_standards_interval_count 0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.760
_exptl_absorpt_correction_T_max  0.962325
_exptl_absorpt_correction_T_min  0.715744
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.329
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             476
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.947
_refine_diff_density_min         -0.506
_refine_diff_density_rms         0.068
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.050
_refine_ls_goodness_of_fit_obs   1.060
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     121
_refine_ls_number_reflns         2895
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.050
_refine_ls_restrained_S_obs      1.060
_refine_ls_R_factor_all          0.0404
_refine_ls_R_factor_obs          0.0326
_refine_ls_shift/esd_max         0.001
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0429P)^2^+0.6065P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0865
_refine_ls_wR_factor_obs         0.0813
_reflns_number_observed          2524
_reflns_number_total             2895
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic991405r_2.cif
_cod_data_source_block           ls12_Compound_4
_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.

'_exptl_absorpt_correction_type' value 'Empirical'
changed to 'empirical' 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 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0429P)^2^+0.6065P] 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^)+(0.0429P)^2^+0.6065P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_database_code               4321129