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_4342515
_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_sum            'C91 H53 Br8 F20 N9 O7'
_chemical_formula_weight         2403.63
_chemical_name_systematic
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 ? 
;
_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             2014-01-23
_audit_creation_method
;
Olex2 1.2
(compiled 2013.12.10 svn.r2850 for OlexSys, GUI svn.r4736)
;
_cell_angle_alpha                68.062(4)
_cell_angle_beta                 80.632(5)
_cell_angle_gamma                80.816(5)
_cell_formula_units_Z            2
_cell_length_a                   14.016(3)
_cell_length_b                   16.678(4)
_cell_length_c                   20.834(5)
_cell_measurement_reflns_used    9826
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.91
_cell_measurement_theta_min      2.801
_cell_volume                     4431.2(18)
_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      99.98
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0660
_diffrn_reflns_av_unetI/netI     0.0709
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            72538
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         1.72
_diffrn_source                   'fine-focus sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.724
_exptl_absorpt_correction_T_max  0.000
_exptl_absorpt_correction_T_min  0.000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.1416 before and 0.0570 after correction.
The Ratio of minimum to maximum transmission is 0.3277.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.801
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             2356
_exptl_crystal_size_max          1.351
_exptl_crystal_size_mid          0.952
_exptl_crystal_size_min          0.822
_platon_squeeze_details
;
One molecule of pentane removed by SQUEEZE
;
_refine_diff_density_max         2.020
_refine_diff_density_min         -1.080
_refine_diff_density_rms         0.118
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1243
_refine_ls_number_reflns         18100
_refine_ls_number_restraints     1214
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.0856
_refine_ls_R_factor_gt           0.0557
_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^)+(0.0476P)^2^+7.1287P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1070
_refine_ls_wR_factor_ref         0.1144
_reflns_number_gt                13040
_reflns_number_total             18124
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic502860g_si_002.cif
_cod_data_source_block           6
_cod_depositor_comments
'Adding full bibliography for 4342513--4342515.cif.'
_cod_database_code               4342515
_olex2_refinement_description
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1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,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
4.a Secondary CH2 refined with riding coordinates:
 C03G(H03K,H03L), C03H(H03M,H03N), C03I(H03O,H03P), C03K(H03Q,H03R), C03N(H03S,
 H03T), C03O(H03U,H03V), C03S(H03W,H03X), C03J(H03Y,H), C03M(H03Z,HA), C03R(H03,
 HB), C03T(H0AA,HC)
4.b Aromatic/amide H refined with riding coordinates:
 C02D(H02D), C02P(H02P), C02U(H02U), C03B(H03B), C018(H018), C022(H022),
 C030(H030), C035(H035), C01D(H01D), C01J(H01J), C01L(H01L), C01S(H01S),
 C01U(H01U), C01Z(H01Z), C02C(H02C), C023(H023)
4.c Idealised Me refined as rotating group:
 C03L(H03A,H03C,H03D), C037(H03E,H03F,H03G), C03F(H03H,H03I,H03J)
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