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_7125462
_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            'C106 H168 N12 Ni O16 S5'
_chemical_formula_weight         2085.53
_space_group_IT_number           96
_space_group_name_Hall           'P 4nw 2abw'
_space_group_name_H-M_alt        'P 43 21 2'
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_H-M   'P 43 21 2'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.091(3)
_cell_length_b                   15.091(3)
_cell_length_c                   63.545(18)
_cell_measurement_temperature    293(2)
_cell_volume                     14472(6)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_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      293(2)
_diffrn_measured_fraction_theta_full 0.936
_diffrn_measured_fraction_theta_max 0.936
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.3052
_diffrn_reflns_av_sigmaI/netI    0.5436
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       70
_diffrn_reflns_limit_l_min       -49
_diffrn_reflns_number            46236
_diffrn_reflns_theta_full        24.30
_diffrn_reflns_theta_max         24.30
_diffrn_reflns_theta_min         5.31
_exptl_absorpt_coefficient_mu    0.257
_exptl_absorpt_correction_type   none
_exptl_crystal_density_diffrn    0.957
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             4496
_refine_diff_density_max         0.558
_refine_diff_density_min         -0.297
_refine_diff_density_rms         0.075
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.05(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.015
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     643
_refine_ls_number_reflns         10825
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.015
_refine_ls_R_factor_all          0.3255
_refine_ls_R_factor_gt           0.1198
_refine_ls_shift/su_max          1.449
_refine_ls_shift/su_mean         0.065
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2650
_refine_ls_wR_factor_ref         0.3091
_reflns_number_gt                2864
_reflns_number_total             10825
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            904134f.txt
_cod_data_source_block           Ni-3
_cod_depositor_comments
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The following automatic conversions were performed:

data item '_symmetry_cell_setting' value 'Tetragonal' was changed to
'tetragonal' in accordance with the
/home/saulius/struct/COD-crude-data/automatic-downloads/DataCite-retrospective/RSC/depositions/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 6909 2019-04-08 15:41:33Z antanas 
;
_cod_original_sg_symbol_H-M      P4(3)2(1)2
_cod_database_code               7125462