A chemoenzymatic synthesis of the carbobicyclic core associated with CP-225,917 and CP-263,114 (phomoidrides A and B)
Banwell, Martin G.; McRae, Kenneth J.; Willis, Anthony C.; Journal of the Chemical Society, Perkin Transactions 1  (2001) 2194–; doi:10.1039/b105376k

data_7216876
_publ_section_title
;
 A chemoenzymatic synthesis of the carbobicyclic core associated with
 CP-225,917 and CP-263,114 (phomoidrides A and B)
;
_journal_issue                   18
_journal_name_full
'Journal of the Chemical Society, Perkin Transactions 1'
_journal_page_first              2194
_journal_paper_doi               10.1039/b105376k
_journal_year                    2001
_chemical_formula_moiety         'C25 H34 O9 '
_chemical_formula_sum            'C25 H34 O9'
_chemical_formula_weight         478.54
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      4
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_audit_creation_date             1999-09-03
_audit_creation_method           'by teXsan v1.8'
_audit_update_record
;
1999-09-03 - Report on C25 H34 O9
by Anthony C. Willis
for Kenneth J. McRae and Martin G. Banwell
2000-11-06 - passes checkcif tests with minor warnings
;
_cell_angle_alpha                90
_cell_angle_beta                 105.15(1)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   9.968(2)
_cell_length_b                   10.083(2)
_cell_length_c                   12.633(1)
_cell_measurement_reflns_used    21
_cell_measurement_temperature    193.2
_cell_measurement_theta_max      54.9
_cell_measurement_theta_min      51.5
_cell_volume                     1225.6(4)
_computing_cell_refinement       'MSC/AFC Diffractometer Control'
_computing_data_collection       'MSC/AFC Diffractometer Control'
_computing_data_reduction        'teXsan (MSC, 1992-1997)'
_computing_publication_material  'teXsan (MSC, 1992-1997)'
_computing_structure_refinement  'teXsan (MSC, 1992-1997)'
_computing_structure_solution
;
SIR92 (Altomare, et. al. 1994)
;
_diffrn_ambient_temperature      193.2
_diffrn_measurement_device_details
;
Rigaku AFC6R diffractometer with extended arm and
evacuated collimator and beam tunnel.
Data cannot be collected beyond \y 60 deg in this configuration.
;
_diffrn_measurement_device_type  'Rigaku AFC6R'
_diffrn_measurement_method       \w-2\q
_diffrn_orient_matrix_UB_11      0.01227
_diffrn_orient_matrix_UB_12      -0.03115
_diffrn_orient_matrix_UB_13      -0.07204
_diffrn_orient_matrix_UB_21      0.10139
_diffrn_orient_matrix_UB_22      0.02122
_diffrn_orient_matrix_UB_23      0.02495
_diffrn_orient_matrix_UB_31      0.01929
_diffrn_orient_matrix_UB_32      -0.09174
_diffrn_orient_matrix_UB_33      0.03023
_diffrn_radiation_detector       'scintillation counter'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Rigaku rotating anode'
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  0.02404
_diffrn_reflns_av_sigmaI/netI    0.040
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            3876
_diffrn_reflns_reduction_process 'Lp corrections applied'
_diffrn_reflns_theta_max         60.15
_diffrn_reflns_theta_min         3.62
_diffrn_standards_decay_%        -0.75
_diffrn_standards_interval_count 150
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.819
_exptl_absorpt_correction_T_max  0.944
_exptl_absorpt_correction_T_min  0.790
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
analytical (de Meulenaer & Tompa, 1965)
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.297
_exptl_crystal_density_meas      ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             512.00
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.44
_refine_diff_density_min         -0.25
_refine_ls_abs_structure_details
;
The absolute configuration has been assigned
on the basis of the known chirality of synthetic precursors.
;
_refine_ls_extinction_coef       0.0000055(3)
_refine_ls_extinction_expression 'equ(3) Acta Cryst.(1968) A24, p213.'
_refine_ls_extinction_method     'Zachariasen (1967)'
_refine_ls_goodness_of_fit_all   2.839
_refine_ls_goodness_of_fit_ref   2.938
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_constraints    15
_refine_ls_number_parameters     332
_refine_ls_number_reflns         1909
_refine_ls_number_restraints     20
_refine_ls_R_factor_all          0.0567
_refine_ls_R_factor_gt           0.0525
_refine_ls_shift/su_max          0.0540
_refine_ls_shift/su_mean         0.0120
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     'w = 1/[\s^2^(Fo) + 0.00022|Fo|^2^]'
_refine_ls_weighting_scheme      sigma
_refine_ls_wR_factor_all         0.0444
_refine_ls_wR_factor_ref         0.0440
_reflns_number_gt                1909
_reflns_number_total             1948
_reflns_threshold_expression     I>2.00\s(I)
_cod_data_source_file            b105376k.txt
_cod_data_source_block           kjm1
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_sg_symbol_H-M      'P 21       '
_cod_original_formula_sum        'C25 H34 O9 '
_cod_database_code               7216876