A monoclinic polymorph of bis(tert-butylperthiophosphonic) dianhydride
Ziemer, Burkhard; Steinberger, Hans-Uwe; Acta Crystallographica Section C Crystal Structure Communications 56 (2000) e95–; doi:10.1107/S0108270100002390

data_2019349
_publ_section_title
;
 A monoclinic polymorph of bis(tert-butylperthiophosphonic) dianhydride
;
_journal_issue                   3
_journal_name_full
'Acta Crystallographica Section C Crystal Structure Communications'
_journal_page_first              e95
_journal_paper_doi               10.1107/S0108270100002390
_journal_volume                  56
_journal_year                    2000
_chemical_formula_moiety         'C8 H18 P2 S4'
_chemical_formula_sum            'C8 H18 P2 S4'
_chemical_formula_weight         304.40
_chemical_name_systematic
;
t-butylperthiophosphonic anhydride
;
_space_group_IT_number           12
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2y'
_symmetry_space_group_name_H-M   'C 1 2/m 1'
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 104.252(8)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   9.7313(8)
_cell_length_b                   9.2898(11)
_cell_length_c                   8.1150(10)
_cell_measurement_reflns_used    62
_cell_measurement_temperature    180(2)
_cell_measurement_theta_max      17.1
_cell_measurement_theta_min      13.0
_cell_volume                     711.03(14)
_computing_cell_refinement       STADI4-1.06
_computing_data_collection       'STADI4-1.06 (Stoe & Cie, 1997)'
_computing_data_reduction        'XRED-1.07 (Stoe & Cie, 1997)'
_computing_publication_material  SHELXL97
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      180(2)
_diffrn_measured_fraction_theta_full .999
_diffrn_measured_fraction_theta_max .999
_diffrn_measurement_device       'Stoe Stadi-4'
_diffrn_measurement_method
'2\q/\w scan, ratio = 1.0, width(\w) = 1.55-1.7\%'
_diffrn_radiation_monochromator  'planar graphite'
_diffrn_radiation_source         'fine-focus sealed X-ray tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     .71073
_diffrn_reflns_av_R_equivalents  .038
_diffrn_reflns_av_sigmaI/netI    .0220
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            3495
_diffrn_reflns_theta_full        27.56
_diffrn_reflns_theta_max         27.56
_diffrn_reflns_theta_min         2.59
_diffrn_standards_decay_%        4.5
_diffrn_standards_interval_time  120
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    .858
_exptl_absorpt_correction_T_max  .808
_exptl_absorpt_correction_T_min  .640
_exptl_absorpt_correction_type   '\y scan'
_exptl_absorpt_process_details   '(North et al., 1968)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.422
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'square plate'
_exptl_crystal_F_000             320
_exptl_crystal_size_max          .57
_exptl_crystal_size_mid          .57
_exptl_crystal_size_min          .26
_refine_diff_density_max         .561
_refine_diff_density_min         -.416
_refine_ls_extinction_coef       .038(3)
_refine_ls_extinction_method     SHELXL97
_refine_ls_goodness_of_fit_ref   1.145
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     59
_refine_ls_number_reflns         876
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.145
_refine_ls_R_factor_all          .025
_refine_ls_R_factor_gt           .025
_refine_ls_shift/su_max          .007
_refine_ls_shift/su_mean         .001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[\s^2^(Fo^2^)+(0.0387P)^2^+0.2726P] where P = (Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         .064
_reflns_number_gt                846
_reflns_number_total             876
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            qb0189sup1.cif
_cod_data_source_block           I
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 
;
_cod_original_cell_volume        711.03(13)
_cod_original_sg_symbol_H-M      'C 2/m'
_cod_database_code               2019349