Synthesis, Characterization, and Reactivity Studies of Subphthalocyanine Boron Triflate
Wang, Zikuan; Fu, Xuefeng; Organometallics 36 (2017) 285–; doi:10.1021/acs.organomet.6b00754

data_4086981
_publ_section_title
;
 Synthesis, Characterization, and Reactivity Studies of Subphthalocyanine
 Boron Triflate
;
_journal_issue                   2
_journal_name_full               Organometallics
_journal_page_first              285
_journal_paper_doi               10.1021/acs.organomet.6b00754
_journal_volume                  36
_journal_year                    2017
_chemical_formula_moiety         'C27 H21 B N6 O Si, 0.5(C2 H5 O), 0.5(H2 O)'
_chemical_formula_sum            'C28 H25 B N6 O2 Si'
_chemical_formula_weight         515.93
_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   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2015-08-13
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_cell_angle_alpha                80.125(8)
_cell_angle_beta                 73.867(6)
_cell_angle_gamma                88.177(10)
_cell_formula_units_Z            4
_cell_length_a                   11.329(3)
_cell_length_b                   12.492(3)
_cell_length_c                   19.268(5)
_cell_measurement_reflns_used    8325
_cell_measurement_temperature    173.1500
_cell_measurement_theta_max      27.4761
_cell_measurement_theta_min      2.4106
_cell_volume                     2580.3(11)
_computing_cell_refinement       'CrystalClear (Rigaku Inc., 2007)'
_computing_data_collection       'CrystalClear (Rigaku Inc., 2007)'
_computing_data_reduction        'CrystalClear (Rigaku Inc., 2007)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution
;
????
;
_diffrn_ambient_temperature      173.1500
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_details
;
scan:
    Number of images: 360
               Slice: -110.0000 - 70.0000
         Image width: 0.5000
            Exp time: 7.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 45.0000
                 Phi: 0.0000
                 XTD: 40.1245
              2theta: -19.9245
scan:
    Number of images: 360
               Slice: -110.0000 - 70.0000
         Image width: 0.5000
            Exp time: 7.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 45.0000
                 Phi: 180.0000
                 XTD: 40.1245
              2theta: -19.9245
scan:
    Number of images: 344
               Slice: -110.0000 - 62.0000
         Image width: 0.5000
            Exp time: 7.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 45.0000
                 Phi: 270.0000
                 XTD: 40.1245
              2theta: -19.9245
;
_diffrn_measurement_device
;
Saturn724+ (2x2 bin mode)
;
_diffrn_measurement_device_details
;
AFC10: Fixed Chi 2 circle
;
_diffrn_measurement_device_type  'multiwire proportional'
_diffrn_measurement_method       dtprofit.ref
_diffrn_orient_matrix_type       d*Trek
_diffrn_orient_matrix_UB_11      0.0064
_diffrn_orient_matrix_UB_12      0.0911
_diffrn_orient_matrix_UB_13      -0.0105
_diffrn_orient_matrix_UB_21      -0.0588
_diffrn_orient_matrix_UB_22      -0.0009
_diffrn_orient_matrix_UB_23      -0.0561
_diffrn_orient_matrix_UB_31      -0.0301
_diffrn_orient_matrix_UB_32      -0.0080
_diffrn_orient_matrix_UB_33      0.0451
_diffrn_radiation_detector       CCD
_diffrn_radiation_monochromator  'Graphite Monochromator'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0428
_diffrn_reflns_av_unetI/netI     0.0503
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            32499
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         27.509
_diffrn_reflns_theta_min         2.233
_diffrn_source                   'Sealed Tube'
_diffrn_source_current           30.0000
_diffrn_source_power             1.5000
_diffrn_source_voltage           50.0000
_exptl_absorpt_coefficient_mu    0.130
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.8615
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.328
_exptl_crystal_description       plate
_exptl_crystal_F_000             1078
_exptl_crystal_size_max          0.78
_exptl_crystal_size_mid          0.68
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.370
_refine_diff_density_min         -0.374
_refine_diff_density_rms         0.056
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.159
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     693
_refine_ls_number_reflns         11782
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.159
_refine_ls_R_factor_all          0.0782
_refine_ls_R_factor_gt           0.0695
_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^)+(0.0611P)^2^+1.8818P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1604
_refine_ls_wR_factor_ref         0.1659
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10588
_reflns_number_total             11782
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om6b00754_si_002.cif
_cod_data_source_block           (subPc)BOTMS
_cod_depositor_comments
;

2020-05-25
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C56 H49 B2 N12 O4 Si2'
_cod_original_formula_weight         1031.87
_cod_original_formula_moiety         '2(C27 H21 B N6 O Si), C2 H5 O, H2 O'
_cod_original_formula_units_Z            2
_cod_original_cell_volume        2580.4(11)
_cod_database_code               4086981
_diffrn_number_total             11788
_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, All O(H) groups, All O(H,H) groups
2.a Riding coordinates:
 O3(H3B,H3C)
2.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C6(H6), C11(H11), C12(H12), C13(H13), C14(H14),
 C19(H19), C20(H20), C21(H21), C22(H22), C3A(H3A), C4A(H4A), C5A(H5A), C6A(H6A),
  C11A(H11A), C12A(H12A), C13A(H13A), C14A(H14A), C19A(H19A), C20A(H20A),
 C21A(H21A), C22A(H22A), C26(H26)
2.c Idealised Me refined as rotating group:
 C0AA(H0AA,H0AB,H0AC), C1AA(H1AA,H1AB,H1AC), C27(H27A,H27B,H27C), C25A(H25A,
 H25B,H25C), C26A(H26A,H26B,H26C), C27A(H27D,H27E,H27F), C25(H25D,H25E,H25F)
2.d Idealised tetrahedral OH refined as rotating group:
 O2(H2)
;
_shelx_res_checksum              3549
_shelx_hkl_checksum              94048
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'