A Porphyrin-Related Macrocycle from Carbazole and Pyridine Building Blocks: Synthesis and Metal Coordination
Lena Arnold; Hassan Norouzi-Arasi; Manfred Wagner; Volker Enkelmann; Klaus Mullen; Chem.Commun. 47 (2011) 970–; doi:10.1039/c0cc03052j

data_7105837
_publ_section_title
;
 A Porphyrin-Related Macrocycle from Carbazole and Pyridine Building
 Blocks: Synthesis and Metal Coordination
;
_journal_name_full               Chem.Commun.
_journal_page_first              970
_journal_paper_doi               10.1039/c0cc03052j
_journal_volume                  47
_journal_year                    2011
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C68 H88 Co1 N4 O5.50'
_chemical_formula_sum            'C68 H88 Co N4 O5.5'
_chemical_formula_weight         1108.40
_space_group_IT_number           18
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2bc 2'
_symmetry_space_group_name_H-M   'P 2 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             10-10-05
_audit_creation_method           CRYSTALS_ver_12.84
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.1483(4)
_cell_length_b                   21.8882(9)
_cell_length_c                   29.7527(9)
_cell_measurement_reflns_used    0
_cell_measurement_temperature    120
_cell_measurement_theta_max      0
_cell_measurement_theta_min      0
_cell_volume                     5957.7(4)
_computing_cell_refinement       'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 1997-2001).'
_computing_data_reduction        'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'CRYSTALS (Betteridge et al., 2003)'
_diffrn_ambient_temperature      120
_diffrn_measured_fraction_theta_full 0.976
_diffrn_measured_fraction_theta_max 0.872
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       '\f & \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.000
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            29056
_diffrn_reflns_theta_full        25.265
_diffrn_reflns_theta_max         27.462
_diffrn_reflns_theta_min         2.508
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.331
_exptl_absorpt_correction_T_max  0.96
_exptl_absorpt_correction_T_min  0.58
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SORTAV (Blessing)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.236
_exptl_crystal_description       prism
_exptl_crystal_F_000             2060
_exptl_crystal_size_max          0.43
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.13
_platon_squeeze_details
;

;
_refine_diff_density_max         0.55
_refine_diff_density_min         -0.62
_refine_ls_abs_structure_details 'Flack (1983), 0 Friedel-pairs'
_refine_ls_abs_structure_Flack   0.086(5)
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.9431
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     619
_refine_ls_number_reflns         9174
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0826
_refine_ls_R_factor_gt           0.0625
_refine_ls_shift/su_max          0.018609
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details
;

Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982)

[weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)]

where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax

Method = Robust Weighting (Prince, 1982)

W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^

A~i~ are:

2.33 1.98 1.09

;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.2536
_refine_ls_wR_factor_gt          0.0630
_refine_ls_wR_factor_ref         0.0630
_reflns_limit_h_max              11
_reflns_limit_h_min              -11
_reflns_limit_k_max              27
_reflns_limit_k_min              0
_reflns_limit_l_max              38
_reflns_limit_l_min              0
_reflns_number_gt                9174
_reflns_number_total             10964
_reflns_threshold_expression     I>2.0\s(I)
_cod_data_source_file            C0CC03052J.TXT
_cod_data_source_block           arnco
_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 
;
_cod_original_sg_symbol_H-M      'P 2 21 21 '
_cod_original_formula_sum        'C68 H88 Co1 N4 O5.50'
_cod_database_code               7105837