Dibenzidecaphyrins (1.0.0.1.1.1.0.0.1.1) and Their Bis-BF<sub>2</sub> Complexes.
Kumar, Sunit; Thorat, Kishor G.; Ravikanth, Mangalampalli; The Journal of organic chemistry 83 (2018) 14277–14285; doi:10.1021/acs.joc.8b01812

data_4035700
_publ_section_title
;
 Dibenzidecaphyrins (1.0.0.1.1.1.0.0.1.1) and Their Bis-BF<sub>2</sub>
 Complexes.
;
_journal_issue                   23
_journal_name_full               'The Journal of organic chemistry'
_journal_page_first              14277
_journal_page_last               14285
_journal_paper_doi               10.1021/acs.joc.8b01812
_journal_volume                  83
_journal_year                    2018
_chemical_formula_moiety         'C51 H39 F5 N2 S2'
_chemical_formula_sum            'C51 H39 F5 N2 S2'
_chemical_formula_weight         838.96
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2018-01-26
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_cell_angle_alpha                90
_cell_angle_beta                 112.258(8)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   25.3837(15)
_cell_length_b                   23.3917(9)
_cell_length_c                   19.2584(16)
_cell_measurement_reflns_used    4021
_cell_measurement_temperature    150
_cell_measurement_theta_max      69.2770
_cell_measurement_theta_min      2.6570
_cell_volume                     10583.0(13)
_computing_cell_refinement
;
CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)
;
_computing_data_collection
;
CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)
;
_computing_data_reduction
;
CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'SIR2004 (Burla et al., 2007)'
_diffrn_ambient_temperature      150
_diffrn_detector_area_resol_mean 28.5714
_diffrn_detector_type            'Rigaku Saturn724+'
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
--------------------------------------------------------------------------
  1  \w   -191.00 -11.00   1.00    4.00    -- -101.00   0.00 108.00  180
  2  \w    -66.00  58.00   1.00    4.00    --  -32.00  72.00 -36.00  124
  3  \w   -112.00 -59.00   1.00    4.00    -- -101.00  72.00  36.00   53
  4  \w   -191.00 -86.00   1.00    4.00    -- -101.00 -72.00-108.00  105
  5  \w   -128.00 -48.00   1.00    4.00    -- -101.00  72.00 -36.00   80
  6  \w   -119.00 -57.00   1.00    4.00    -- -101.00  72.00-180.00   62
  7  \w   -115.00 -47.00   1.00    4.00    --  -32.00   0.00-180.00   68
  8  \w    -97.00 -67.00   1.00    4.00    -- -101.00 -72.00-180.00   30
  9  \w    -44.00 -12.00   1.00    4.00    -- -101.00  72.00 108.00   32
 10  \w   -191.00 -67.00   1.00    4.00    -- -101.00 -72.00 -36.00  124
 11  \w   -115.00 -11.00   1.00    4.00    -- -101.00  72.00-108.00  104
 12  \w   -122.00   2.00   1.00    4.00    --  -32.00 -72.00 -36.00  124
;
_diffrn_measurement_device       'AFC12 (Right): Kappa 3 circle'
_diffrn_measurement_device_type  'Rigaku Saturn724+ (2x2 bin mode)'
_diffrn_measurement_method       'profile data from \w-scans'
_diffrn_measurement_specimen_support 'Mitegen 50um'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.1524
_diffrn_reflns_av_unetI/netI     0.1079
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            35904
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        64.998
_diffrn_reflns_theta_max         64.998
_diffrn_reflns_theta_min         2.666
_exptl_absorpt_coefficient_mu    1.314
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.38138
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
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    1.053
_exptl_crystal_description       block
_exptl_crystal_F_000             3488
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.071
_refine_diff_density_max         0.500
_refine_diff_density_min         -0.362
_refine_diff_density_rms         0.078
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.008
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     547
_refine_ls_number_reflns         8970
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.008
_refine_ls_R_factor_all          0.1592
_refine_ls_R_factor_gt           0.0947
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1585P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2512
_refine_ls_wR_factor_ref         0.3119
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4459
_reflns_number_total             8970
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            jo8b01812_si_002.cif
_cod_data_source_block           mr-sk-mtbu-pf-2_cu_sq
_cod_database_code               4035700
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.912
_shelx_estimated_absorpt_t_min   0.694
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 N2(H2), C18(H18), C17(H17), C28(H28), C29(H29), C2(H2A), C7(H7), C3(H3),
 C8(H8), C40(H40), C43(H43), C14(H14), C51(H51), C15(H15), C44(H44), C41(H41),
 C33(H33), C34(H34), C47(H47), C49(H49), C48(H48)
2.b Idealised Me refined as rotating group:
 C38(H38A,H38B,H38C), C37(H37A,H37B,H37C), C39(H39A,H39B,H39C), C13(H13A,H13B,
 H13C), C11(H11A,H11B,H11C), C12(H12A,H12B,H12C)
;
_shelx_res_checksum              31915
_shelx_hkl_checksum              81292
_shelx_fab_checksum              19271
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
- Detector area scaling
;