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_4022340
_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         ' C60 H93 N3 Ni1 O2 Si3 '
_chemical_formula_sum            'C60 H93 N3 Ni O2 Si3'
_chemical_formula_weight         1031.39
_chemical_melting_point          ?
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   18.0619(2)
_cell_length_b                   22.7317(3)
_cell_length_c                   29.3777(4)
_cell_measurement_reflns_used    12480
_cell_measurement_temperature    150
_cell_measurement_theta_max      25
_cell_measurement_theta_min      4
_cell_volume                     12061.8(3)
_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_max 0.992
_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  0.05
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            24074
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         5.12
_diffrn_standards_decay_%        0.00
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.423
_exptl_absorpt_correction_T_max  0.98
_exptl_absorpt_correction_T_min  0.96
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
  Denzo/Scalepack (Otwinowski & Minor, 1996)
;
_exptl_crystal_colour            ' blue '
_exptl_crystal_density_diffrn    1.136
_exptl_crystal_density_meas      ?
_exptl_crystal_description       ' plate '
_exptl_crystal_F_000             4485.205
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.47
_refine_diff_density_min         -0.29
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.0750
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     622
_refine_ls_number_reflns         6442
_refine_ls_R_factor_gt           0.0451
_refine_ls_shift/su_max          0.013738
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details
;
  Method= Tukey and Prince
  W = [weight] * [1-(deltaF/6*sigmaF)^2]^2
  1.62 -0.276 0.923
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.0476
_reflns_limit_h_max              22
_reflns_limit_h_min              0
_reflns_limit_k_max              28
_reflns_limit_k_min              0
_reflns_limit_l_max              36
_reflns_limit_l_min              0
_reflns_number_gt                6442
_reflns_number_total             12224
_reflns_threshold_expression     >2.50\s(I)
_cod_data_source_file            jo026748csi20021121_094930_9.cif
_cod_data_source_block           compound_Ni7
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Orthorhombic ' changed to 'orthorhombic'
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 b c a '
_cod_original_formula_sum        ' C60 H93 N3 Ni1 O2 Si3 '
_cod_database_code               4022340