Transition-Metal-Mediated [2 + 2 + 2] Cycloaddition Reactions with Ethyne-Containing Porphyrin Templates: New Routes to Cofacial Porphyrin Structures and Facially-Functionalized (Porphinato)metal Species
James T. Fletcher; Michael J. Therien; Journal of the American Chemical Society 122 (2000) 12393–12394; doi:10.1021/ja0001557

data_4116263
_publ_section_title
;
 Transition-Metal-Mediated [2 + 2 + 2] Cycloaddition Reactions with
 Ethyne-Containing Porphyrin Templates: New Routes to Cofacial Porphyrin
 Structures and Facially-Functionalized (Porphinato)metal Species
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              12393
_journal_page_last               12394
_journal_paper_doi               10.1021/ja0001557
_journal_volume                  122
_journal_year                    2000
_chemical_formula_sum            'C71 H78 N8 O6 Zn2'
_chemical_formula_weight         1270.15
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 109.350(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.5885(5)
_cell_length_b                   27.5919(10)
_cell_length_c                   16.7882(8)
_cell_measurement_reflns_used    25940
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      25.35
_cell_measurement_theta_min      0.0
_cell_volume                     5938.9(4)
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SIR92 (Altomare, 1992)'
_diffrn_ambient_temperature      120(2)
_diffrn_measurement_device_type  'Rigaku R-AXIS IIc Area Detector'
_diffrn_measurement_method       'image plate \f oscillations'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0717
_diffrn_reflns_av_sigmaI/netI    0.0533
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            34107
_diffrn_reflns_theta_max         25.35
_diffrn_reflns_theta_min         2.54
_exptl_absorpt_coefficient_mu    0.871
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            red-brown
_exptl_crystal_density_diffrn    1.421
_exptl_crystal_description       plate
_exptl_crystal_F_000             2672
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.966
_refine_diff_density_min         -0.656
_refine_diff_density_rms         0.078
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.238
_refine_ls_goodness_of_fit_obs   1.299
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     807
_refine_ls_number_reflns         10215
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.238
_refine_ls_restrained_S_obs      1.299
_refine_ls_R_factor_all          0.1364
_refine_ls_R_factor_obs          0.1146
_refine_ls_shift/esd_max         -0.010
_refine_ls_shift/esd_mean        0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0284P)^2^+29.4155P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.2095
_refine_ls_wR_factor_obs         0.1988
_reflns_number_observed          8442
_reflns_number_total             10215
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ja0001557.cif
_cod_data_source_block           shelxl
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0284P)^2^+29.4155P] where P=(Fo^2^+2Fc^2^)/3'
was changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0284P)^2^+29.4155P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_sg_symbol_H-M      'P 21/c '
_cod_database_code               4116263