High-yield synthesis of a chiroporphyrin by hydrogen bond-directed cyclisation
Pérollier, Céline; Pécaut, Jacques; Ramasseul, René; Marchon, Jean-Claude; Bau, Robert; Chemical Communications  (1999) 1597–; doi:10.1039/a904134f

data_7125461
_publ_section_title
;
 High-yield synthesis of a chiroporphyrin by hydrogen bond-directed
 cyclisation
;
_journal_issue                   16
_journal_name_full               'Chemical Communications'
_journal_page_first              1597
_journal_paper_doi               10.1039/a904134f
_journal_year                    1999
_chemical_formula_sum            'C20 H32 N2 O3'
_chemical_formula_weight         348.48
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.861(2)
_cell_length_b                   20.595(3)
_cell_length_c                   8.948(2)
_cell_measurement_temperature    163
_cell_volume                     2001.5(6)
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0922
_diffrn_reflns_av_sigmaI/netI    0.0526
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -1
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -1
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_limit_l_min       -1
_diffrn_reflns_number            1574
_diffrn_reflns_theta_max         50.72
_diffrn_reflns_theta_min         2.29
_exptl_absorpt_coefficient_mu    0.615
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.156
_exptl_crystal_description       needle
_exptl_crystal_F_000             760
_exptl_crystal_size_max          0.55
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.268
_refine_diff_density_min         -0.246
_refine_diff_density_rms         0.054
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.27(180)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.187
_refine_ls_goodness_of_fit_obs   1.929
_refine_ls_matrix_type           full
_refine_ls_number_parameters     226
_refine_ls_number_reflns         1421
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.305
_refine_ls_restrained_S_obs      1.929
_refine_ls_R_factor_all          0.0667
_refine_ls_R_factor_obs          0.0608
_refine_ls_shift/esd_max         -0.027
_refine_ls_shift/esd_mean        0.005
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.2659P)^2^+9.7118P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1882
_refine_ls_wR_factor_obs         0.1553
_reflns_number_observed          1287
_reflns_number_total             1425
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            904134f.txt
_cod_data_source_block           2
_cod_depositor_comments
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The following automatic conversions were performed:

data item '_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.2659P)^2^+9.7118P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. A new data item '_refine_ls_weighting_details' was
created with the value set to
'w=1/[\s^2^(Fo^2^)+(0.2659P)^2^+9.7118P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 6909 2019-04-08 15:41:33Z antanas 
;
_cod_database_code               7125461