Synthesis of meso-Tetraaryl Triphyrins(2.1.1).
Panda, Kamakshya Nath; Thorat, Kishor G.; Ravikanth, Mangalampalli; The Journal of organic chemistry 83 (2018) 12945–12950; doi:10.1021/acs.joc.8b02242

data_4035417
_publ_section_title
;
 Synthesis of meso-Tetraaryl Triphyrins(2.1.1).
;
_journal_issue                   20
_journal_name_full               'The Journal of organic chemistry'
_journal_page_first              12945
_journal_page_last               12950
_journal_paper_doi               10.1021/acs.joc.8b02242
_journal_volume                  83
_journal_year                    2018
_chemical_formula_moiety         'C40 H27 N3'
_chemical_formula_sum            'C40 H27 N3'
_chemical_formula_weight         556.26
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-I 2ya'
_space_group_name_H-M_alt        'I 1 2/a 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2018-03-08
_audit_creation_method
;
Olex2 1.2-ac3
(compiled 2016.08.26 svn.r3337 for Rigaku Oxford Diffraction, GUI svn.r5221)
;
_cell_angle_alpha                90
_cell_angle_beta                 110.991(10)
_cell_angle_gamma                90
_cell_formula_units_Z            16
_cell_length_a                   40.424(4)
_cell_length_b                   6.9876(5)
_cell_length_c                   44.765(4)
_cell_measurement_reflns_used    14457
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      30.8650
_cell_measurement_theta_min      1.8790
_cell_volume                     11805(2)
_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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 CCD
_diffrn_detector_area_resol_mean 28.5714
_diffrn_detector_type            'Rigaku Saturn724+'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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   -110.00   9.50   0.50    8.00    --  -20.00 -72.00-180.00  239
  2  \w    -69.00  19.00   0.50    8.00    --  -20.00 -72.00  36.00  176
  3  \w    -59.00  60.50   0.50    8.00    --  -20.00  72.00 -36.00  239
  4  \w    -59.00  70.00   0.50    8.00    --  -20.00  72.00  36.00  258
  5  \w    -87.00  19.00   0.50    8.00    --  -20.00 -72.00-108.00  212
  6  \w   -110.00  -7.50   0.50    8.00    --  -20.00 -72.00 108.00  205
  7  \w    -85.00 -13.00   0.50    8.00    --  -20.00 -72.00 -36.00  144
  8  \w     32.00  70.00   0.50    8.00    --  -20.00   0.00 108.00   76
  9  \w     -5.00  70.00   0.50    8.00    --  -20.00  72.00-108.00  150
 10  \w    -59.00  70.00   0.50    8.00    --  -20.00  72.00-180.00  258
 11  \w    -18.00  70.00   0.50    8.00    --  -20.00  72.00 108.00  176
 12  \w     16.00  59.50   0.50    8.00    --  -20.00   0.00 -36.00   87
 13  \w   -110.00  70.00   0.50    8.00    --  -20.00   0.00-180.00  360
 14  \w   -110.00  66.00   0.50    8.00    --  -20.00   0.00  36.00  352
;
_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_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0169664000
_diffrn_orient_matrix_UB_12      0.0109261000
_diffrn_orient_matrix_UB_13      -0.0011063000
_diffrn_orient_matrix_UB_21      0.0057533000
_diffrn_orient_matrix_UB_22      0.0526178000
_diffrn_orient_matrix_UB_23      0.0145159000
_diffrn_orient_matrix_UB_31      0.0056702000
_diffrn_orient_matrix_UB_32      -0.0861027000
_diffrn_orient_matrix_UB_33      0.0087275000
_diffrn_radiation_collimation    0.3
_diffrn_radiation_monochromator  Confocal
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.3744
_diffrn_reflns_av_unetI/netI     0.1389
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       48
_diffrn_reflns_limit_h_min       -48
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       53
_diffrn_reflns_limit_l_min       -53
_diffrn_reflns_number            155709
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        24.999
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_min         1.693
_diffrn_source                   'Rotating Anode'
_diffrn_source_current           24.0
_diffrn_source_power             1.2
_diffrn_source_target            Mo
_diffrn_source_type              'Rotating Anode'
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    0.073
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.30894
_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            red
_exptl_crystal_density_diffrn    1.237
_exptl_crystal_description       trapizium
_exptl_crystal_F_000             4608
_exptl_crystal_size_max          0.235
_exptl_crystal_size_mid          0.144
_exptl_crystal_size_min          0.025
_refine_diff_density_max         0.395
_refine_diff_density_min         -0.462
_refine_diff_density_rms         0.126
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     775
_refine_ls_number_reflns         10393
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.1803
_refine_ls_R_factor_gt           0.0912
_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^)+(0.1000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1990
_refine_ls_wR_factor_ref         0.2471
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5034
_reflns_number_total             10393
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            jo8b02242_si_004.cif
_cod_data_source_block           mr-kp-phtriphyrin_mo
_cod_depositor_comments
;

2020-10-09
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_cell_volume        11805.4(19)
_cod_original_formula_moiety     '0.31(C40 H27 N3)'
_cod_original_formula_sum        'C12.55 H8.47 N0.94'
_cod_original_formula_units_Z    51
_cod_original_formula_weight     172.44
_cod_database_code               4035417
_shelx_shelxl_version_number     2014/7
_exptl_absorpt_special_details   good
_reflns_odcompleteness_completeness 95.96
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     31.11
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 N005(H005), N006(H006), C007(H007), C009(H009), C00A(H00A), C00B(H00B),
 C00C(H00C), C00E(H00E), C00N(H00N), C00Q(H00Q), C00R(H00R), C00T(H00T),
 C00V(H00V), C010(H010), C013(H013), C014(H014), C015(H015), C017(H017),
 C018(H018), C01A(H01A), C01C(H01C), C01D(H01D), C01F(H01F), C01G(H01G),
 C01I(H01I), C01J(H01J), C01K(H01K), C01L(H01L), C01M(H01M), C01P(H01P),
 C01Q(H01Q), C01R(H01R), C01S(H01S), C01U(H01U), C01V(H01V), C01W(H01W),
 C01X(H01X), C01Y(H01Y), C01Z(H01Z), C020(H020), C021(H021), C022(H022),
 C023(H023), C024(H024), C025(H025), C026(H026), C027(H027), C028(H028),
 C029(H029), C02A(H02A), C02B(H02B), C02C(H02C), C02D(H02D), C02E(H02E)
;
_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
;
_oxdiff_exptl_absorpt_empirical_full_max 7.383
_oxdiff_exptl_absorpt_empirical_full_min 0.349