Core-modified 48π and 42π decaphyrins: syntheses, properties and structures
Ghosh, Arindam; Dash, Syamasrit; Srinivasan, A.; Suresh, C. H.; Peruncheralathan, S.; Chandrashekar, Tavarekere K.; Organic Chemistry Frontiers 6 (2019) 3746–; doi:10.1039/C9QO01162E

data_1555209
_publ_section_title
;
 Core-modified 48\p and 42\p decaphyrins: syntheses, properties and
 structures
;
_journal_issue                   22
_journal_name_full               'Organic Chemistry Frontiers'
_journal_page_first              3746
_journal_paper_doi               10.1039/C9QO01162E
_journal_volume                  6
_journal_year                    2019
_chemical_formula_moiety         '0.3(C148 H128 N4 S6)'
_chemical_formula_sum            'C44.4 H38.4 N1.2 S1.8'
_chemical_formula_weight         646.47
_space_group_crystal_system      hexagonal
_space_group_IT_number           180
_space_group_name_Hall           'P 62 2 (0 0 4)'
_space_group_name_H-M_alt        'P 62 2 2'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2018-02-03
_audit_creation_method
;
Olex2 1.2-alpha
(compiled 2016.02.24 svn.r3266 for OlexSys, GUI svn.r5155)
;
_audit_update_record
;
2019-01-05 deposited with the CCDC.	2019-09-30 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            20
_cell_length_a                   28.8585(6)
_cell_length_b                   28.8585(6)
_cell_length_c                   37.6170(4)
_cell_measurement_reflns_used    19727
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      71.6090
_cell_measurement_theta_min      2.9020
_cell_volume                     27130.8(8)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.0
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.971
_diffrn_measurement_device_type
'SuperNova, Dual, Cu at home/near, Pilatus 200K'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_unetI/netI     0.0636
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.971
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       46
_diffrn_reflns_limit_l_min       -46
_diffrn_reflns_number            18453
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.959
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         77.407
_diffrn_reflns_theta_min         2.940
_exptl_absorpt_coefficient_mu    0.971
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.67427
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.29d (Rigaku Oxford Diffraction, 2017)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    0.791
_exptl_crystal_description       needle
_exptl_crystal_F_000             6840
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.182
_refine_diff_density_min         -0.147
_refine_diff_density_rms         0.023
_refine_ls_abs_structure_details
;
 Flack x determined using 3450 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.037(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.828
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     725
_refine_ls_number_reflns         18452
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.828
_refine_ls_R_factor_all          0.0697
_refine_ls_R_factor_gt           0.0421
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0536P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0947
_refine_ls_wR_factor_ref         0.1041
_reflns_Friedel_coverage         0.777
_reflns_Friedel_fraction_full    0.998
_reflns_Friedel_fraction_max     0.944
_reflns_number_gt                10585
_reflns_number_total             18452
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9qo01162e2.cif
_cod_data_source_block           tkc_homo_penta
_cod_original_cell_volume        27130.8(12)
_cod_original_sg_symbol_Hall     'P 62 2c (0 0 1)'
_cod_original_formula_sum        'C44.40 H38.40 N1.20 S1.80'
_cod_database_code               1555209
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C13(H13), C22(H22), C23(H23), C10(H10), C43(H43), C18(H18), C25(H25), C9(H9),
 C68(H68), C17(H17), C70(H70), C27(H27), C5(H5), C45(H45), C59(H59), C4(H4),
 C61(H61), C56(H56), C52(H52), C29(H29), C28(H28), C31(H31), C55(H55), C53(H53),
  C54(H54), C30(H30), C36(H36), C34(H34)
2.b Idealised Me refined as rotating group:
 C47(H47A,H47B,H47C), C64(H64A,H64B,H64C), C48(H48A,H48B,H48C), C63(H63A,H63B,
 H63C), C73(H73A,H73B,H73C), C72(H72A,H72B,H72C), C74(H74A,H74B,H74C), C65(H65A,
 H65B,H65C), C49(H49A,H49B,H49C), C38(H38A,H38B,H38C), C39(H39A,H39B,H39C),
 C40(H40A,H40B,H40C)
;
_shelx_res_checksum              52072
_shelx_hkl_checksum              10763
_shelx_shelxl_version_number     2016/4
_olex2_submission_special_instructions 'No special instructions were received'