Synthesis and crystal structure of a meso-trialkynyl-[28]hexaphyrinThis is one of a number of contributions from the current members of the Dyson Perrins Laboratory to mark the end of almost 90 years of organic chemistry research in that building, as all its current academic staff move across South Parks Road to a new purpose-built laboratory.
Krivokapic, Alexander; Anderson, Harry L.; Organic & Biomolecular Chemistry 1 (2003) 3639–; doi:10.1039/b306725b

data_7151507
_publ_section_title
;
 Synthesis and crystal structure of a
 meso-trialkynyl-[28]hexaphyrinThis is one of a number of contributions
 from the current members of the Dyson Perrins Laboratory to mark the
 end of almost 90 years of organic chemistry research in that building,
 as all its current academic staff move across South Parks Road to a
 new purpose-built laboratory.
;
_journal_issue                   21
_journal_name_full               'Organic &amp;  Biomolecular Chemistry'
_journal_page_first              3639
_journal_paper_doi               10.1039/b306725b
_journal_volume                  1
_journal_year                    2003
_chemical_compound_source
;
?
;
_chemical_formula_moiety         ' C112 H111 Cl3 N6 Si3 '
_chemical_formula_sum            'C112 H111 Cl3 N6 Si3'
_chemical_formula_weight         1731.77
_chemical_melting_point          ?
_chemical_name_systematic
;
?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yab'
_symmetry_space_group_name_H-M   'P 1 21/a 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_cell_angle_alpha                90
_cell_angle_beta                 99.019(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   32.9322(14)
_cell_length_b                   8.6290(4)
_cell_length_c                   36.665(2)
_cell_measurement_reflns_used    5765
_cell_measurement_temperature    150
_cell_measurement_theta_max      21
_cell_measurement_theta_min      3
_cell_volume                     10290.3(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
;
SIR97 (Altomare et al, 1999)
;
_diffrn_ambient_temperature      150
_diffrn_measured_fraction_theta_full 0.933
_diffrn_measured_fraction_theta_max 0.785
_diffrn_measurement_device_type
;
Enraf Nonius Kappa CCD
;
_diffrn_measurement_method       \w/2\q
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.04
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            13445
_diffrn_reflns_theta_full        15.751
_diffrn_reflns_theta_max         20.932
_diffrn_reflns_theta_min         2.975
_diffrn_standards_decay_%        0.00
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.173
_exptl_absorpt_correction_T_max  0.99
_exptl_absorpt_correction_T_min  0.98
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
Denzo/Scalepack (Otwinowski & Minor, 1996)
;
_exptl_crystal_colour            ' blue '
_exptl_crystal_density_diffrn    1.118
_exptl_crystal_density_meas      ?
_exptl_crystal_description       ' plate '
_exptl_crystal_F_000             3672.000
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.32
_refine_diff_density_min         -0.65
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.9523
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1087
_refine_ls_number_reflns         6813
_refine_ls_R_factor_all          0.2122
_refine_ls_R_factor_gt           0.1833
_refine_ls_shift/su_max          0.043178
_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

3.81 2.73 2.71 0.465
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.2016
_refine_ls_wR_factor_gt          0.1626
_refine_ls_wR_factor_ref         0.1611
_reflns_limit_h_max              30
_reflns_limit_h_min              -31
_reflns_limit_k_max              8
_reflns_limit_k_min              0
_reflns_limit_l_max              36
_reflns_limit_l_min              0
_reflns_number_gt                6858
_reflns_number_total             8605
_reflns_threshold_expression     I>1.00u(I)
_cod_data_source_file            b306725b.txt
_cod_data_source_block           compound_Hexaphyrin
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic ' changed to 'monoclinic'
according to '/home/adriana/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 1555 2011-01-17 13:19:09Z 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 1569 2011-02-09 13:29:24Z adriana 
;
_cod_original_cell_volume        10290.4(9)
_cod_original_sg_symbol_H-M      'P 1 21/a 1 '
_cod_original_formula_sum        ' C112 H111 Cl3 N6 Si3 '
_cod_database_code               7151507