Key Intermediates in the Synthesis of 2,2'-Biphosphole
Tissot, Olivier; Gouygou, Maryse; Daran, Jean-Claude; Balavoine, Gilbert; Acta Crystallographica Section C 54 (1998) 676–679; doi:10.1107/S0108270197018179

data_2007276
_publ_section_title
;
 Key Intermediates in the Synthesis of 2,2'-Biphosphole
;
_journal_issue                   5
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              676
_journal_page_last               679
_journal_paper_doi               10.1107/S0108270197018179
_journal_volume                  54
_journal_year                    1998
_chemical_formula_moiety         ' C12 H12 Br P S '
_chemical_formula_sum            'C12 H12 Br P S'
_chemical_formula_weight         299.16
_chemical_name_systematic
;
 1-phenyl-2-bromo-3,4-dimethylphosphole sulfide
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_cell_angle_alpha                92.61(2)
_cell_angle_beta                 96.96(2)
_cell_angle_gamma                109.53(2)
_cell_formula_units_Z            2
_cell_length_a                   7.3535(15)
_cell_length_b                   7.9457(17)
_cell_length_c                   11.731(2)
_cell_measurement_reflns_used    3713
_cell_measurement_temperature    180(2)
_cell_measurement_theta_max      24.27
_cell_measurement_theta_min      2.73
_cell_volume                     638.5(2)
_computing_cell_refinement       'IPDS software'
_computing_data_collection       'IPDS software (Stoe, 1996a)'
_computing_data_reduction        'X-RED (Stoe, 1996b)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'
_computing_publication_material  SHELXL97
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_diffrn_ambient_temperature      180(2)
_diffrn_measured_fraction_theta_full 0.899
_diffrn_measured_fraction_theta_max 0.899
_diffrn_measurement_device_type  'Stoe IPDS'
_diffrn_measurement_method       '\f rotation'
_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  0.0526
_diffrn_reflns_av_sigmaI/netI    0.0161
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
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_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            3713
_diffrn_reflns_theta_full        24.27
_diffrn_reflns_theta_max         24.27
_diffrn_reflns_theta_min         2.73
_diffrn_standards_decay_%        negligible
_diffrn_standards_interval_count 'Area detector used'
_diffrn_standards_interval_time  'Area detector used'
_diffrn_standards_number         '200 for each image'
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_exptl_absorpt_correction_T_max  0.311
_exptl_absorpt_correction_T_min  0.157
_exptl_absorpt_correction_type   'numerical (Stoe, 1996c)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.556
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
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_exptl_crystal_size_min          0.42
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_refine_ls_extinction_method     none
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_refine_ls_matrix_type           full
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_refine_ls_number_reflns         1866
_refine_ls_number_restraints     0
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_refine_ls_R_factor_all          0.0427
_refine_ls_R_factor_gt           0.0364
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0411P)^2^+1.8879P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_obs         .0950
_refine_ls_wR_factor_ref         0.0997
_reflns_number_gt                1611
_reflns_number_total             1866
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            sk1134.cif
_cod_data_source_block           4
_cod_depositor_comments
;
The following automatic conversions were performed:
'_geom_bond_publ_flag' value 'YES' changed to 'yes' according to
'/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29 (8 times).

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_geom_bond_publ_flag' value 'YES' changed to 'yes' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29 (8
times).

'_geom_angle_publ_flag' value 'YES' changed to 'yes'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29 (16
times).

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc w =
1/[\s^2^(Fo^2^)+(0.0411P)^2^+1.8879P] 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^)+(0.0411P)^2^+1.8879P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_formula_sum        ' C12 H12 Br P S '
_cod_database_code               2007276