Benzyl 5-{2-[2-(diethoxyphosphinoyl)acetyl]-3-oxo-7-thia-2,4-diazabicyclo[3.3.0]oct-6-yl}pentanoate, a novel biotin derivative
Amspacher, David R.; Blanchard, Carol Z.; Saraiva, Marcelo C.; Waldrop, Grover L.; Strongin, Robert M.; Fronczek, Frank R.; Acta Crystallographica Section C 56 (2000) e305–e306; doi:10.1107/S0108270100007915

data_2011172
_publ_section_title
;Benzyl
 5-{2-[2-(diethoxyphosphinoyl)acetyl]-3-oxo-7-thia-2,4-diazabicyclo[3.3.0]oct-6-yl}pentanoate,
 a novel biotin derivative
;
_journal_issue                   7
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              e305
_journal_page_last               e306
_journal_paper_doi               10.1107/S0108270100007915
_journal_volume                  56
_journal_year                    2000
_chemical_formula_moiety         'C23 H33 N2 O7 P S'
_chemical_formula_sum            'C23 H33 N2 O7 P S'
_chemical_formula_weight         512.57
_chemical_name_systematic
;
phenylmethyl 5-(6,8-diaza-6-(2-diethoxyphosphono)
acetyl)-7-oxo-3-thiabicyclo [3.3.0] oct-2-yl) pentanoate
;
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_cell_angle_alpha                90
_cell_angle_beta                 115.077(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   10.455(2)
_cell_length_b                   12.410(2)
_cell_length_c                   10.592(2)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    100
_cell_measurement_theta_max      18.2
_cell_measurement_theta_min      8.9
_cell_volume                     1244.7(4)
_computing_cell_refinement       'CAD-4 EXPRESS'
_computing_data_collection       'CAD-4 EXPRESS (Enraf-Nonius, 1994)'
_computing_data_reduction        'PROCESS in MolEN (Fair, 1990)'
_computing_publication_material  'CIFTAB in SHELXL97'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'direct methods using SIR (Burla et al., 1989)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full .997
_diffrn_measured_fraction_theta_max .997
_diffrn_measurement_device
'Enraf-Nonius CAD-4 (with Oxford Cryostreams Cryostream cooler)'
_diffrn_measurement_method       \q/2\q
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         sealed_tube
_diffrn_radiation_type           Mo-K\a
_diffrn_radiation_wavelength     .71073
_diffrn_reflns_av_R_equivalents  .033
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            5600
_diffrn_reflns_theta_full        30.0
_diffrn_reflns_theta_max         30.0
_diffrn_reflns_theta_min         2.5
_diffrn_standards_decay_%        2.9
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    .24
_exptl_absorpt_correction_T_max  .959
_exptl_absorpt_correction_T_min  .920
_exptl_absorpt_correction_type   '\y scan'
_exptl_absorpt_process_details   '(North et al., 1968)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.368
_exptl_crystal_density_method    none
_exptl_crystal_description       prism
_exptl_crystal_F_000             544
_exptl_crystal_size_max          .50
_exptl_crystal_size_mid          .33
_exptl_crystal_size_min          .18
_refine_diff_density_max         .44
_refine_diff_density_min         -.43
_refine_ls_abs_structure_details 'Flack (1983)'
_refine_ls_abs_structure_Flack   '-0.07(8); 1521 Friedel pairs'
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.12
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     309
_refine_ls_number_reflns         5297
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.12
_refine_ls_R_factor_all          .057
_refine_ls_R_factor_gt           .040
_refine_ls_shift/su_max          .002
_refine_ls_shift/su_mean         .000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[\s^2^(Fo^2^)+(0.0378P)^2^+0.6507P] where P = (Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         .101
_reflns_number_gt                4521
_reflns_number_total             5297
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            qa0325.cif
_cod_data_source_block           I
_cod_original_sg_symbol_Hall     'P 2y1'
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               2011172
_cod_database_fobs_code          2011172