Photophysical Properties of β-Substituted Free-Base Corroles.
Lemon, Christopher M.; Halbach, Robert L.; Huynh, Michael; Nocera, Daniel G.; Inorganic chemistry 54 (2015) 2713–2725; doi:10.1021/ic502860g

data_4342514
_publ_section_title
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 Photophysical Properties of \b-Substituted Free-Base Corroles.
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_journal_issue                   6
_journal_name_full               'Inorganic chemistry'
_journal_page_first              2713
_journal_page_last               2725
_journal_paper_doi               10.1021/ic502860g
_journal_volume                  54
_journal_year                    2015
_chemical_formula_moiety         'C78 H34 F20 N8 O4'
_chemical_formula_sum            'C78 H34 F20 N8 O4'
_chemical_formula_weight         1527.14
_chemical_name_systematic
;
 ? 
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_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_date             2014-01-21
_audit_creation_method
;
Olex2 1.2
(compiled 2013.11.15 svn.r2834 for OlexSys, GUI svn.r4709)
;
_cell_angle_alpha                96.489(13)
_cell_angle_beta                 114.139(12)
_cell_angle_gamma                105.927(12)
_cell_formula_units_Z            2
_cell_length_a                   16.198(13)
_cell_length_b                   17.515(14)
_cell_length_c                   17.649(14)
_cell_measurement_reflns_used    7360
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      22.59
_cell_measurement_theta_min      2.24
_cell_volume                     4247(6)
_computing_cell_refinement       'SAINT 7.46A (Bruker-AXS, 2009)'
_computing_data_collection       'APEX2 v2009.3.0 (Bruker-AXS, 2009)'
_computing_data_reduction        'SAINT 7.46A (Bruker-AXS, 2009)'
_computing_molecular_graphics    'Bruker SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'Bruker SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      99.99
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0850
_diffrn_reflns_av_unetI/netI     0.0981
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            50877
_diffrn_reflns_theta_full        23.53
_diffrn_reflns_theta_max         23.53
_diffrn_reflns_theta_min         1.25
_diffrn_source                   'fine-focus sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.105
_exptl_absorpt_correction_T_max  0.992
_exptl_absorpt_correction_T_min  0.952
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.194
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Plate
_exptl_crystal_F_000             1540
_exptl_crystal_size_max          0.641
_exptl_crystal_size_mid          0.389
_exptl_crystal_size_min          0.074
_platon_squeeze_details
;
Three THF molecules and one molecule of pentane removed by SQUEEZE.
;
_refine_diff_density_max         0.425
_refine_diff_density_min         -0.439
_refine_diff_density_rms         0.059
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.935
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     925
_refine_ls_number_reflns         12583
_refine_ls_number_restraints     1365
_refine_ls_restrained_S_all      0.889
_refine_ls_R_factor_all          0.1302
_refine_ls_R_factor_gt           0.0698
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1141P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1812
_refine_ls_wR_factor_ref         0.2053
_reflns_number_gt                6464
_reflns_number_total             12596
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic502860g_si_002.cif
_cod_data_source_block           3
_cod_depositor_comments
'Adding full bibliography for 4342513--4342515.cif.'
_cod_database_code               4342514
_olex2_refinement_description
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1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Rigid bond restraints
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 1.7A with sigma of 0.04 and sigma
for terminal atoms of 0.08
Uanis(C45) = Uanis(C46) = Uanis(C47) = Uanis(C48) = Uanis(C49) = Uanis(C50) =
Uanis(C45A) = Uanis(C46A) = Uanis(C47A) = Uanis(C48A) = Uanis(C49A) =
Uanis(C50A)
Uanis(F11) = Uanis(F12) = Uanis(F13) = Uanis(F14) = Uanis(F15) = Uanis(F11A) =
Uanis(F12A) = Uanis(F13A) = Uanis(F14A) = Uanis(F15A)
4. Others
 Sof(C45A)=Sof(C46A)=Sof(C47A)=Sof(C48A)=Sof(C49A)=Sof(C50A)=Sof(F11A)=
 Sof(F12A)=Sof(F13A)=Sof(F14A)=Sof(F15A)=1-FVAR(1)
 Sof(C45)=Sof(C46)=Sof(C47)=Sof(C48)=Sof(C49)=Sof(C50)=Sof(F11)=Sof(F12)=
 Sof(F13)=Sof(F14)=Sof(F15)=FVAR(1)
5.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C13(H13), C14(H14), C18(H18), C19(H19), C23(H23), C24(H24), C26(H26),
 C27(H27), C37(H37), C38(H38), C41(H41), C42(H42), C52(H52), C53(H53), C63(H63),
  C62(H62), C58(H58), C57(H57), C65(H65), C66(H66), C77(H77), N1(H1), N2(H2A),
 N4(H4), N5(H5), N7(H7), N8(H8)
5.b Fitted hexagon refined as free rotating group:
 C45(C46,C47,C48,C49,C50), C45A(C46A,C47A,C48A,C49A,C50A), C56(C63,C62,C59,C58,
 C57), C69(C74,C73,C72,C71,C70)
5.c Idealised Me refined as rotating group:
 C22(H22A,H22B,H22C), C61(H61A,H61B,H61C)
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