Oligomers of a 5-carboxy-methanopyrrolidine β-amino acid. A search for order.
Krow, Grant R.; Liu, Nian; Sender, Matthew; Lin, Guoliang; Centafont, Ryan; Sonnet, Philip E.; DeBrosse, Charles; Ross, 3rd, Charles W; Carroll, Patrick J.; Shoulders, Matthew D.; Raines, Ronald T.; Organic letters 12 (2010) 5438–5441; doi:10.1021/ol1022917

data_1503304
_publ_section_title
;
 Oligomers of a 5-carboxy-methanopyrrolidine \b-amino acid. A search for
 order.
;
_journal_issue                   23
_journal_name_full               'Organic letters'
_journal_page_first              5438
_journal_page_last               5441
_journal_paper_doi               10.1021/ol1022917
_journal_volume                  12
_journal_year                    2010
_chemical_absolute_configuration rm
_chemical_formula_sum            'C30 H40 N4 O7'
_chemical_formula_weight         568.67
_space_group_IT_number           5
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      5
_symmetry_space_group_name_Hall  'C 2y'
_symmetry_space_group_name_H-M   'C 1 2 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 110.722(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   23.844(6)
_cell_length_b                   6.1411(12)
_cell_length_c                   23.447(5)
_cell_measurement_temperature    143(1)
_cell_volume                     3211.2(12)
_computing_data_collection       'CrystalClear (Rigaku, 1999)'
_computing_data_reduction        'CrystalClear (Rigaku, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR97 (Altomare, 1999)'
_diffrn_ambient_temperature      143(1)
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device       'CCD Area Detector'
_diffrn_measurement_device_type  'Rigaku Mercury'
_diffrn_measurement_method       'phi and omega rotations'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0542
_diffrn_reflns_av_sigmaI/netI    0.0654
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            9821
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.74
_exptl_absorpt_coefficient_mu    0.257
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.4761
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_density_diffrn    1.371
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1404
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.01
_platon_squeeze_details
;
The asymmetric unit includes a molecule of methylene chloride and
one-half of a water molecule. These solvent molecules were disordered;
a reliable disorder model could not be devised. The X-ray data were 
corrected for the presence of disordered solvent by SQUEEZE
;
_refine_diff_density_max         0.466
_refine_diff_density_min         -0.251
_refine_diff_density_rms         0.072
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   1(2)
_refine_ls_extinction_coef       0.0056(13)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     372
_refine_ls_number_reflns         3092
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.0848
_refine_ls_R_factor_gt           0.0742
_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^)+(0.1236P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1802
_refine_ls_wR_factor_ref         0.1886
_reflns_number_gt                2493
_reflns_number_total             3092
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ol1022917_si_004.cif
_cod_data_source_block           shelxl
_cod_depositor_comments
;
The following automatic conversions were performed:
'_atom_site_symetry_multiplicity' tag replaced with
'_atom_site_symmetry_multiplicity'.

Automatic conversion script
Id: cif_correct_tags 1440 2010-10-19 06:21:57Z saulius 

The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'Multi-scan' changed to
'multi-scan' 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 1715 2011-07-08 13:25:40Z adriana 

2017-03-17
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_cell_volume        3211.3(12)
_cod_original_sg_symbol_H-M      'C 2      '
_cod_original_formula_sum        'C62 H86 Cl4 N8 O15'
_cod_original_formula_units_Z    2
_cod_original_formula_weight     1325.19
_cod_database_code               1503304