Phosphorus complexes of a triply-fused [24]pentaphyrin
Higashino, Tomohiro; Osuka, Atsuhiro; Chemical Science 3 (2012) 103–; doi:10.1039/c1sc00653c

data_1515274
_publ_section_title
;
 Phosphorus complexes of a triply-fused [24]pentaphyrin
;
_journal_issue                   1
_journal_name_full               'Chemical Science'
_journal_page_first              103
_journal_paper_doi               10.1039/c1sc00653c
_journal_volume                  3
_journal_year                    2012
_chemical_formula_moiety
'C55 H8 F24 N5 O P, C2 H3 N, 0.75(C Cl4), 0.5(O) '
_chemical_formula_sum            'C57.75 H11 Cl3 F24 N6 O1.5 P'
_chemical_formula_weight         1405.92
_chemical_name_systematic
;
?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_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
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                85.568(3)
_cell_angle_beta                 88.271(3)
_cell_angle_gamma                76.766(3)
_cell_formula_units_Z            2
_cell_length_a                   10.1849(5)
_cell_length_b                   14.9773(8)
_cell_length_c                   17.6759(10)
_cell_measurement_reflns_used    11301
_cell_measurement_temperature    93(2)
_cell_measurement_theta_max      68.09
_cell_measurement_theta_min      3.04
_cell_volume                     2616.7(2)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      93(2)
_diffrn_detector_area_resol_mean 10.0
_diffrn_measured_fraction_theta_full 0.972
_diffrn_measured_fraction_theta_max 0.972
_diffrn_measurement_device_type  'RIGAKU RAXIS-RAPID'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54187
_diffrn_reflns_av_R_equivalents  0.1076
_diffrn_reflns_av_sigmaI/netI    0.1437
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            21103
_diffrn_reflns_theta_full        59.99
_diffrn_reflns_theta_max         59.99
_diffrn_reflns_theta_min         3.04
_exptl_absorpt_coefficient_mu    3.150
_exptl_absorpt_correction_T_max  0.8584
_exptl_absorpt_correction_T_min  0.5714
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.784
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1387
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.615
_refine_diff_density_min         -0.658
_refine_diff_density_rms         0.114
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.076
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     857
_refine_ls_number_reflns         7529
_refine_ls_number_restraints     8
_refine_ls_restrained_S_all      1.077
_refine_ls_R_factor_all          0.1922
_refine_ls_R_factor_gt           0.1190
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2902
_refine_ls_wR_factor_ref         0.3747
_reflns_number_gt                3480
_reflns_number_total             7529
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c1sc00653c.txt
_cod_data_source_block           0901hi
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to
/usr/data/users/saulius/automatic-downloads/retrospective/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 
;
_cod_original_sg_symbol_H-M      P-1
_cod_original_formula_sum        'C57.75 H11 Cl3 F24 N6 O1.50 P'
_cod_database_code               1515274