Synthesis of Oxacalixarene-Locked Bisporphyrins and Higher Oligomers
Erhong Hao; Frank R. Fronczek; M. Graça H. Vicente; Journal of Organic Chemistry 71 (2006) 1233–1236; doi:10.1021/jo051964h

data_4021431
_publ_section_title
;
 Synthesis of Oxacalixarene-Locked Bisporphyrins and Higher Oligomers
;
_journal_name_full               'Journal of Organic Chemistry'
_journal_page_first              1233
_journal_page_last               1236
_journal_paper_doi               10.1021/jo051964h
_journal_volume                  71
_journal_year                    2006
_chemical_compound_source        'local laboratory'
_chemical_formula_moiety         'C100 H60 N12 O12, 5(C H Cl3), H2 O'
_chemical_formula_sum            'C105 H67 Cl15 N12 O13'
_chemical_formula_weight         2236.46
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_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
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90
_cell_angle_beta                 102.191(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   25.122(3)
_cell_length_b                   12.103(2)
_cell_length_c                   33.724(5)
_cell_measurement_reflns_used    13363
_cell_measurement_temperature    110
_cell_measurement_theta_max      23.5
_cell_measurement_theta_min      2.5
_cell_volume                     10023(3)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'COLLECT (Nonius, 2000)'
_computing_data_reduction
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_molecular_graphics    'ORTEP-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR97 (Altomare  et al., 1999)'
_diffrn_ambient_temperature      110
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device       'KappaCCD (with Oxford Cryostream)'
_diffrn_measurement_method       ' \w scans with \k offsets'
_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  0.037
_diffrn_reflns_av_sigmaI/netI    0.0609
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            55817
_diffrn_reflns_theta_full        23.6
_diffrn_reflns_theta_max         23.6
_diffrn_reflns_theta_min         2.6
_diffrn_standards_decay_%        <2
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.482
_exptl_absorpt_correction_T_max  0.931
_exptl_absorpt_correction_T_min  0.812
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'HKL Scalepack (Otwinowski & Minor 1997)'
_exptl_crystal_colour            'dark red-brown'
_exptl_crystal_density_diffrn    1.482
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             4560
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.15
_refine_diff_density_max         2.87
_refine_diff_density_min         -1.60
_refine_diff_density_rms         0.143
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   2.544
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1278
_refine_ls_number_reflns         14806
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      2.544
_refine_ls_R_factor_all          0.177
_refine_ls_R_factor_gt           0.135
_refine_ls_shift/su_max          0.008
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.359
_refine_ls_wR_factor_ref         0.378
_reflns_number_gt                10184
_reflns_number_total             14806
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            jo051964hsi20050919_044811.cif
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_sg_symbol_H-M      'P 21/c        '
_cod_database_code               4021431