({-})-(2<i>R</i>,3<i>R</i>)-<i>O</i>,<i>O</i>'-Dibenzoyl-(2<i>R</i>,3<i>R</i>)-tartaric acid‒hexamethylphosphoramide (1/2)
Yi-Jian Zhang; Shu Zhan; Wen-Jie Feng; Mei-Chao Li; Zhi-Min Jin; Acta Crystallographica Section E 63 (2007) o1546–o1548; doi:10.1107/S1600536807008380

data_2212875
_publ_section_title
;({-})-(2<i>R</i>,3<i>R</i>)-<i>O</i>,<i>O</i>'-Dibenzoyl-(2<i>R</i>,3<i>R</i>)-tartaric
 acid--hexamethylphosphoramide (1/2)
;
_journal_coeditor_code           GK2052
_journal_issue                   4
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o1546
_journal_page_last               o1548
_journal_paper_doi               10.1107/S1600536807008380
_journal_volume                  63
_journal_year                    2007
_chemical_formula_iupac          'C18 H14 O8, 2C6 H18 N3 O P'
_chemical_formula_moiety         'C18 H14 O8, 2(C6 H18 N3 O P)'
_chemical_formula_sum            'C30 H50 N6 O10 P2'
_chemical_formula_weight         716.70
_chemical_name_systematic
;(-)-(2R,3R)-O,O'-Dibenzoyl-(2R,3R)-tartaric acid--hexamethylphosphoramide
 (1/2)
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   12.2940(2)
_cell_length_b                   19.1370(3)
_cell_length_c                   32.5842(6)
_cell_measurement_reflns_used    72558
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      27.51
_cell_measurement_theta_min      3.00
_cell_volume                     7666.1(2)
_computing_cell_refinement       PROCESS-AUTO
_computing_data_collection       'PROCESS-AUTO (Rigaku, 1998)'
_computing_data_reduction        'CrystalStructure (Rigaku/MSC, 2004)'
_computing_molecular_graphics    'SHELXTL (Bruker, 1998)'
_computing_publication_material  SHELXTL
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      571(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID'
_diffrn_measurement_method       \w
_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  0.0175
_diffrn_reflns_av_sigmaI/netI    0.0143
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       41
_diffrn_reflns_limit_l_min       -42
_diffrn_reflns_number            75480
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         3.00
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.171
_exptl_absorpt_correction_T_max  0.9301
_exptl_absorpt_correction_T_min  0.8955
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   '(SHELXTL; Bruker, 1998)'
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.242
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             3056
_exptl_crystal_size_max          0.66
_exptl_crystal_size_mid          0.60
_exptl_crystal_size_min          0.43
_refine_diff_density_max         0.648
_refine_diff_density_min         -0.351
_refine_ls_abs_structure_details 'Flack  (1983), 7969 Friedel pairs'
_refine_ls_abs_structure_Flack   -0.01(4)
_refine_ls_extinction_coef       0.00144(18)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL97
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     905
_refine_ls_number_reflns         17538
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0361
_refine_ls_R_factor_gt           0.0351
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0611P)^2^+1.9189P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0976
_refine_ls_wR_factor_ref         0.0985
_reflns_number_gt                16986
_reflns_number_total             17538
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            gk2052.cif
_cod_data_source_block           I
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Orthorhombic' changed to 'orthorhombic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

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

The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Orthorhombic' changed to
'orthorhombic' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_database_code               2212875
_cod_database_fobs_code          2212875