Contracted and Expanded meso-Alkynyl Porphyrinoids: from Triphyrin to Hexaphyrin
Alexander Krivokapic; Andrew R. Cowley; Harry L. Anderson; Journal of Organic Chemistry 68 (2003) 1089–1096; doi:10.1021/jo026748c

data_4022338
_publ_section_title
;
 Contracted and Expanded meso-Alkynyl Porphyrinoids:
 from Triphyrin to Hexaphyrin
;
_journal_name_full               'Journal of Organic Chemistry'
_journal_page_first              1089
_journal_page_last               1096
_journal_paper_doi               10.1021/jo026748c
_journal_volume                  68
_journal_year                    2003
_chemical_compound_source
;
Synthesised as described.
;
_chemical_formula_moiety         '(C80 H124 N4 Ni1 Si4), (C2 H2 Cl4) '
_chemical_formula_sum            'C82 H126 Cl4 N4 Ni Si4'
_chemical_formula_weight         1480.75
_chemical_melting_point          ?
_chemical_name_systematic
;
?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_cell_angle_alpha                77.8713(5)
_cell_angle_beta                 89.7279(6)
_cell_angle_gamma                63.8827(7)
_cell_formula_units_Z            2
_cell_length_a                   15.4377(2)
_cell_length_b                   17.0745(2)
_cell_length_c                   18.5033(2)
_cell_measurement_reflns_used    18196
_cell_measurement_temperature    150
_cell_measurement_theta_max      27
_cell_measurement_theta_min      1
_cell_volume                     4260.11(9)
_computing_cell_refinement
;
  Denzo/Scalepack (Otwinowski & Minor, 1996)
;
_computing_data_collection
;
  COLLECT (Nonius BV, 1997)
;
_computing_data_reduction
;
  Denzo/Scalepack (Otwinowski & Minor, 1996)
;
_computing_molecular_graphics
;
  CAMERON (Watkin et al 1996)
;
_computing_publication_material
;
  CRYSTALS (Watkin et al 2001)
;
_computing_structure_refinement
;
  CRYSTALS (Watkin et al 2001)
;
_computing_structure_solution
;
  SIR92 (Altomare et al, 1994)
;
_diffrn_ambient_temperature      150
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type
;
Enraf Nonius Kappa CCD
;
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.02
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            35871
_diffrn_reflns_theta_full        27.466
_diffrn_reflns_theta_max         27.466
_diffrn_reflns_theta_min         1.365
_diffrn_standards_decay_%        0.00
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.439
_exptl_absorpt_correction_T_max  0.92
_exptl_absorpt_correction_T_min  0.92
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
  Denzo/Scalepack (Otwinowski & Minor, 1996)
;
_exptl_crystal_colour            ' green '
_exptl_crystal_density_diffrn    1.142
_exptl_crystal_density_meas      ?
_exptl_crystal_description       ' block '
_exptl_crystal_F_000             1580.043
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         1.27
_refine_diff_density_min         -0.69
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.0496
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     934
_refine_ls_number_reflns         11203
_refine_ls_R_factor_all          0.0990
_refine_ls_R_factor_gt           0.0506
_refine_ls_shift/su_max          0.047540
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details
;
Method = Prince modified Chebychev polynomial, (Watkin, 1994)
  W = [weight] * [1-(deltaF/6*sigmaF)^2]^2
  0.815 0.476 0.444
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1148
_refine_ls_wR_factor_gt          0.0599
_refine_ls_wR_factor_ref         0.0598
_reflns_limit_h_max              20
_reflns_limit_h_min              -19
_reflns_limit_k_max              22
_reflns_limit_k_min              -21
_reflns_limit_l_max              24
_reflns_limit_l_min              0
_reflns_number_gt                11262
_reflns_number_total             19394
_reflns_threshold_expression     I>3.00u(I)
_cod_data_source_file            jo026748csi20021121_094930_7.cif
_cod_data_source_block           compound_Ni2
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic ' changed to 'triclinic'
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 

The following automatic conversions were performed:

'_chemical_melting_point' value 'not measured' was changed to '?' -
the value is undefined or not given.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_original_sg_symbol_H-M      'P -1 '
_cod_original_formula_sum        ' C82 H126 Cl4 N4 Ni1 Si4 '
_cod_database_code               4022338