Synthesis of organocatalysts using non-covalent chemistry; understanding the reactivity of ProNap, an enamine-type organocatalyst that can self assemble with complementary co-catalysts
Fuentes, José A.; Lebl, Tomas; Slawin, Alexandra M. Z.; Clarke, Matthew L.; Chemical Science 2 (2011) 1997–; doi:10.1039/c1sc00299f

data_1515481
_publ_section_title
;
 Synthesis of organocatalysts using non-covalent chemistry; understanding
 the reactivity of ProNap, an enamine-type organocatalyst that can self
 assemble with complementary co-catalysts
;
_journal_issue                   10
_journal_name_full               'Chemical Science'
_journal_page_first              1997
_journal_paper_doi               10.1039/c1sc00299f
_journal_volume                  2
_journal_year                    2011
_chemical_absolute_configuration syn
_chemical_formula_moiety         'C15 H18 N4 O,C14 H18 N4 O'
_chemical_formula_sum            'C29 H36 N8 O2'
_chemical_formula_weight         528.66
_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'
_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                 95.440(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.022(5)
_cell_length_b                   10.006(2)
_cell_length_c                   17.448(4)
_cell_measurement_reflns_used    2983
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      68.6
_cell_measurement_theta_min      21.4
_cell_volume                     2784.6(12)
_computing_cell_refinement       'CrystalClear (Rigaku Corp., 2004)'
_computing_data_collection       'CrystalClear (Rigaku Corp., 2004)'
_computing_data_reduction        'CrystalClear (Rigaku Corp., 2004)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.946
_diffrn_measured_fraction_theta_max 0.939
_diffrn_measurement_device_type  CCD
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  confocal
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0599
_diffrn_reflns_av_sigmaI/netI    0.0473
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            36923
_diffrn_reflns_theta_full        67.00
_diffrn_reflns_theta_max         67.96
_diffrn_reflns_theta_min         2.54
_exptl_absorpt_coefficient_mu    0.664
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.835
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.261
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Platelet
_exptl_crystal_F_000             1128
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.432
_refine_diff_density_min         -0.256
_refine_diff_density_rms         0.047
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.4(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     739
_refine_ls_number_reflns         9376
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.065
_refine_ls_R_factor_all          0.0727
_refine_ls_R_factor_gt           0.0588
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0796P)^2^+0.9272P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1480
_refine_ls_wR_factor_ref         0.1645
_reflns_number_gt                7826
_reflns_number_total             9376
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c1sc00299f.txt
_cod_data_source_block           ProNap(12)
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to
/usr/data/users/saulius/automatic-downloads/retrospective/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 
;
_cod_original_sg_symbol_H-M      P2(1)
_cod_database_code               1515481