Tetrathiafulvalene-annulated [28]hexaphyrin(1.1.1.1.1.1): a multi-electron donor system subject to conformational control
Atanu Jana; Masatoshi Ishida; Kevin Cho; Sudip Kumar Ghosh; Kyuju Kwak; Kei Ohkubo; Young Mo Sung; Christina M. Davis; Vincent M. Lynch; Dongil Lee; Shunichi Fukuzumi; Dongho Kim; Jonathan L. Sessle; Chem.Commun. 49 (2013) 8937–; doi:10.1039/c3cc44934c

data_7109806
_publ_section_title
;
 Tetrathiafulvalene-annulated [28]hexaphyrin(1.1.1.1.1.1): a
 multi-electron donor system subject to conformational control
;
_journal_name_full               Chem.Commun.
_journal_page_first              8937
_journal_paper_doi               10.1039/c3cc44934c
_journal_volume                  49
_journal_year                    2013
_chemical_formula_moiety
'C114 H28 N6 F30 S24, 1.7 C H Cl3, 1.7 C4 H10 O'
_chemical_formula_sum            'C122.5 H46.7 Cl5.1 F30 N6 O1.7 S24'
_chemical_formula_weight         3149.79
_chemical_melting_point          428
_chemical_name_common            Benzo-TTF-Hexaphyrin
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 104.276(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   20.732(2)
_cell_length_b                   24.908(2)
_cell_length_c                   28.820(3)
_cell_measurement_reflns_used    111866
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      2.0
_cell_volume                     14423(2)
_computing_cell_refinement       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_collection       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_reduction        'CrystalClear (Rigaku Inc., 2008)'
_computing_molecular_graphics    'XP SHELXTL/PC, Siemens Analytical'
_computing_structure_refinement  'XL SHELXTL/PC, Siemens Analytical'
_computing_structure_solution
;

SIR97 - Altomare A., Burla M.C., Camalli M., Cascarano G.L., Giacovazzo C., 
Guagliardi A., Moliterni A.G.G., Polidori G.,Spagna R.
;
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Rigaku AFC-12 with Saturn 724+ CCD'
_diffrn_measurement_method       \w-scans
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0883
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            12694
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         3.06
_exptl_absorpt_coefficient_mu    0.538
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.416
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
Abscor. T. Higashi (2001). The Rigaku Corporation, Tokyo, Japan.
;
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.451
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prisms
_exptl_crystal_F_000             6312
_exptl_crystal_size_max          0.39
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.09
_platon_squeeze_details
;
;
_refine_diff_density_max         0.536
_refine_diff_density_min         -0.295
_refine_diff_density_rms         0.095
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.985
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1065
_refine_ls_number_reflns         12694
_refine_ls_number_restraints     1542
_refine_ls_restrained_S_all      1.009
_refine_ls_R_factor_all          0.1224
_refine_ls_R_factor_gt           0.0800
_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^)+(0.1450P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2103
_refine_ls_wR_factor_ref         0.2338
_reflns_number_gt                7428
_reflns_number_total             12694
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3cc44934c.txt
_cod_data_source_block           shelxl
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               7109806