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_4035416
_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         '2(C45 H30 N3 O3 Re)'
_chemical_formula_sum            'C90 H60 N6 O6 Re2'
_chemical_formula_weight         1693.84
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2018-05-22
_audit_creation_method
;
Olex2 1.2-ac3
(compiled 2016.08.26 svn.r3337 for Rigaku Oxford Diffraction, GUI svn.r5221)
;
_cell_angle_alpha                82.049(2)
_cell_angle_beta                 83.907(2)
_cell_angle_gamma                78.263(2)
_cell_formula_units_Z            2
_cell_length_a                   15.6837(4)
_cell_length_b                   15.8931(4)
_cell_length_c                   16.9110(5)
_cell_measurement_reflns_used    10566
_cell_measurement_temperature    150
_cell_measurement_theta_max      30.8120
_cell_measurement_theta_min      1.7300
_cell_volume                     4074.22(19)
_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)'
_diffrn_ambient_temperature      150
_diffrn_detector                 CCD
_diffrn_detector_area_resol_mean 28.5714
_diffrn_detector_type            'Rigaku Saturn724+'
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_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  19.00   0.50    8.00    --  -20.00 -72.00  36.00  258
  2  \w    -92.50  19.00   0.50    8.00    --  -20.00 -72.00-108.00  223
  3  \w   -107.00  -0.50   0.50    8.00    --  -20.00   0.00-108.00  213
;
_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      -0.0120744000
_diffrn_orient_matrix_UB_12      -0.0317518000
_diffrn_orient_matrix_UB_13      -0.0198959000
_diffrn_orient_matrix_UB_21      -0.0435105000
_diffrn_orient_matrix_UB_22      0.0237307000
_diffrn_orient_matrix_UB_23      0.0001721000
_diffrn_orient_matrix_UB_31      0.0104191000
_diffrn_orient_matrix_UB_32      0.0231678000
_diffrn_orient_matrix_UB_33      -0.0375414000
_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  0.0906
_diffrn_reflns_av_unetI/netI     0.1215
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            27439
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        24.999
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_min         1.684
_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    3.023
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.56155
_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            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.381
_exptl_crystal_description       needle
_exptl_crystal_F_000             1680
_exptl_crystal_size_max          0.077
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.016
_refine_diff_density_max         0.875
_refine_diff_density_min         -1.663
_refine_diff_density_rms         0.203
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     941
_refine_ls_number_reflns         14210
_refine_ls_number_restraints     60
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.0831
_refine_ls_R_factor_gt           0.0551
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0424P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1176
_refine_ls_wR_factor_ref         0.1359
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10034
_reflns_number_total             14210
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            jo8b02242_si_003.cif
_cod_data_source_block           mr-kp-retoltriphyrin4a_mo_sq
_cod_database_code               4035416
_shelx_shelxl_version_number     2014/7
_reflns_odcompleteness_completeness 85.33
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     31.13
_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. Uiso/Uaniso restraints and constraints
Uanis(C00L) \\sim Ueq, Uanis(C016) \\sim Ueq, Uanis(C01Q) \\sim Ueq,
Uanis(C00Z) \\sim Ueq, Uanis(C02C) \\sim Ueq, Uanis(C01H) \\sim Ueq,
Uanis(C017) \\sim Ueq, Uanis(C01L) \\sim Ueq, Uanis(C01R) \\sim Ueq,
Uanis(C00Q) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.001
3.a Aromatic/amide H refined with riding coordinates:
 C00D(H00D), C00H(H00H), C00O(H00O), C00P(H00P), C00R(H00R), C00X(H00X),
 C011(H011), C012(H012), C015(H015), C018(H018), C019(H019), C01A(H01A),
 C01C(H01C), C01D(H01D), C01E(H01E), C01F(H01F), C01G(H01G), C01K(H01K),
 C01N(H01N), C01O(H01O), C01Q(H01Q), C01U(H01U), C01V(H01V), C01X(H01X),
 C01Z(H01Z), C020(H020), C021(H021), C024(H024), C025(H025), C026(H026),
 C027(H027), C028(H028), C029(H029), C02E(H02G), C02F(H02H), C02I(H02M),
 C02J(H02J), C02N(H02N), C02O(H02O), C02P(H02P), C02R(H02R), C02W(H02W),
 C02X(H02X), C030(H030), C032(H032), C1(H1), C2(H2), C3(H3)
3.b Idealised Me refined as rotating group:
 C02H(H02I,H02K,H02L), C02Q(H02A,H02B,H02C), C02V(H02D,H02E,H02F), C031(H03A,
 H03B,H03C)
;
_shelx_fab_checksum              64077
_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
;
_oxdiff_exptl_absorpt_empirical_full_max 1.664
_oxdiff_exptl_absorpt_empirical_full_min 0.771