Acetylenic scaffolding with subphthalocyanines ‒ synthetic scope and elucidation of electronic interactions in dimeric structures
Gotfredsen, Henrik; Broløs, Line; Holmstrøm, Thomas; Sørensen, Jacob; Viñas, Alberto; Kilde, Martin Drøhse; Skov, Anders B.; Santella, Marco; Hammerich, Ole; Nielsen, Mogens Brøndsted; Org. Biomol. Chem.  (2017) –; doi:10.1039/C7OB01907F

data_7155908
_publ_section_title
;
 Acetylenic scaffolding with subphthalocyanines -- synthetic scope and
 elucidation of electronic interactions in dimeric structures
;
_journal_name_full               'Org. Biomol. Chem.'
_journal_paper_doi               10.1039/C7OB01907F
_journal_year                    2017
_chemical_formula_moiety         'B2 C76 H66 N12 Si2'
_chemical_formula_sum            'C76 H66 B2 N12 Si2'
_chemical_formula_weight         1158.75
_chemical_name_systematic        'SubPc dimer'
_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_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_primary     iterative
_audit_creation_date             2017-09-18
_audit_creation_method
;
Olex2 1.2
(compiled 2017.07.20 svn.r3457 for OlexSys, GUI svn.r5370)
;
_audit_update_record
;
2017-09-18 deposited with the CCDC.
2017-10-02 downloaded from the CCDC.
;
_cell_angle_alpha                86.111(5)
_cell_angle_beta                 73.453(5)
_cell_angle_gamma                87.487(6)
_cell_formula_units_Z            2
_cell_length_a                   13.474(2)
_cell_length_b                   14.769(2)
_cell_length_c                   19.430(3)
_cell_measurement_reflns_used    9474
_cell_measurement_temperature    296.15
_cell_measurement_theta_max      62.052
_cell_measurement_theta_min      5.526
_cell_volume                     3696.6(9)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine (Bourhis et al., 2015)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 0.9877
_diffrn_measured_fraction_theta_max 0.9877
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0878
_diffrn_reflns_av_unetI/netI     0.0533
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            84253
_diffrn_reflns_theta_full        25.0273
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         2.07
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.094
_exptl_absorpt_correction_T_max  0.7462
_exptl_absorpt_correction_T_min  0.6685
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.1536 before and 0.0901 after correction.
The Ratio of minimum to maximum transmission is 0.8959.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.0409
_exptl_crystal_description       Prism
_exptl_crystal_F_000             1156.7508
_exptl_crystal_size_max          0.641
_exptl_crystal_size_mid          0.44
_exptl_crystal_size_min          0.202
_refine_diff_density_max         0.9976
_refine_diff_density_min         -0.6728
_refine_diff_density_rms         0.1291
_refine_ls_d_res_high            0.8400
_refine_ls_d_res_low             9.8355
_refine_ls_goodness_of_fit_ref   0.8395
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     829
_refine_ls_number_reflns         12889
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.8395
_refine_ls_R_factor_all          0.1102
_refine_ls_R_factor_gt           0.0935
_refine_ls_shift/su_max          0.0007
_refine_ls_shift/su_mean         0.0002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1939P)^2^+27.0205P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2717
_refine_ls_wR_factor_ref         0.2985
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              16
_reflns_limit_h_min              -15
_reflns_limit_k_max              17
_reflns_limit_k_min              -17
_reflns_limit_l_max              23
_reflns_limit_l_min              0
_reflns_number_gt                10149
_reflns_number_total             12889
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            c7ob01907f2.cif
_cod_data_source_block           mo_D8V1605_0m-1
_cod_original_cell_volume        3696.8(10)
_cod_original_formula_sum        'B2 C76 H66 N12 Si2'
_cod_database_code               7155908
_olex2_refinement_description
;
;
_olex2_submission_special_instructions 'No special instructions were received'