Covalently linked meso-tetraaryl triphyrin(2.1.1)-ferrocene(s) conjugates: synthesis and properties.
Panda, Kamakshya Nath; Thorat, Kishor G.; Ravikanth, Mangalampalli; Organic & biomolecular chemistry 17 (2019) 5066–5074; doi:10.1039/c9ob00647h

data_7156811
_publ_section_title
;
 Covalently linked meso-tetraaryl triphyrin(2.1.1)-ferrocene(s)
 conjugates: synthesis and properties.
;
_journal_issue                   20
_journal_name_full               'Organic &amp; biomolecular chemistry'
_journal_page_first              5066
_journal_page_last               5074
_journal_paper_doi               10.1039/c9ob00647h
_journal_volume                  17
_journal_year                    2019
_chemical_formula_moiety         'C56 H43 Fe N3'
_chemical_formula_sum            'C56 H43 Fe N3'
_chemical_formula_weight         813.826
_chemical_name_common            dyad
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2018-12-31
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2018-12-31 deposited with the CCDC.    2019-04-26 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 94.387(8)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.3859(10)
_cell_length_b                   17.6141(10)
_cell_length_c                   22.8451(19)
_cell_measurement_reflns_used    5281
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      28.2930
_cell_measurement_theta_min      2.1410
_cell_volume                     4167.0(6)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_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 plate'
_diffrn_detector_area_resol_mean 28.5714
_diffrn_detector_type            'Rigaku Saturn724+'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.917
_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  53.00   0.50    8.00    --  -20.00   0.00  36.00  326
  2  \w    -63.00 -33.00   0.50    8.00    --  -20.00   0.00 -36.00   60
  3  \w    -18.00  69.00   0.50    8.00    --  -20.00  72.00 -36.00  174
  4  \w     -9.00  21.50   0.50    8.00    --  -20.00  72.00 108.00   61
  5  \w   -110.00  70.00   0.50    8.00    --  -20.00   0.00-108.00  360
  6  \w    -98.00 -65.00   0.50    8.00    --  -20.00 -72.00-108.00   66
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type
'dtrek-CrysAlisPro-abstract goniometer imported rigaku-d*trek images'
_diffrn_measurement_method       '\w scans'
_diffrn_measurement_specimen_support 'Mitegen 50um'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0568187000
_diffrn_orient_matrix_UB_12      -0.0212118000
_diffrn_orient_matrix_UB_13      -0.0077979000
_diffrn_orient_matrix_UB_21      -0.0036886000
_diffrn_orient_matrix_UB_22      0.0164177000
_diffrn_orient_matrix_UB_23      -0.0284095000
_diffrn_orient_matrix_UB_31      0.0381569000
_diffrn_orient_matrix_UB_32      -0.0300092000
_diffrn_orient_matrix_UB_33      -0.0100708000
_diffrn_radiation_collimation    0.3
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.2662
_diffrn_reflns_av_unetI/netI     0.3106
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.917
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            56659
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.917
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.193
_diffrn_reflns_theta_min         1.788
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_current           24.0
_diffrn_source_power             1.2
_diffrn_source_target            Mo
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    0.405
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.58600
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.292
_exptl_crystal_F_000             1692
_exptl_crystal_size_max          0.116
_exptl_crystal_size_mid          0.106
_exptl_crystal_size_min          0.048
_refine_diff_density_max         1.259
_refine_diff_density_min         -0.870
_refine_diff_density_rms         0.188
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.106
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     545
_refine_ls_number_reflns         12392
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.106
_refine_ls_R_factor_all          0.4362
_refine_ls_R_factor_gt           0.1807
_refine_ls_shift/su_max          0.151
_refine_ls_shift/su_mean         0.012
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3922
_refine_ls_wR_factor_ref         0.5288
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3150
_reflns_number_total             12392
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9ob00647h2.cif
_cod_data_source_block           mr-kgt-617_mo
_cod_depositor_comments          'Adding full bibliography for 7156811.cif.'
_cod_database_code               7156811
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         C20H20N2
_reflns_odcompleteness_completeness 91.69
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     31.12
_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 Ternary CH refined with riding coordinates:
 C20(H20), C24(H24)
2.b Aromatic/amide H refined with riding coordinates:
 N1(H1), C2(H2), C13(H13), C3(H3), C44(H44), C41(H41), C30(H30), C45(H45),
 C33(H33), C40(H40), C31(H31), C34(H34), C37(H37), C12(H12), C7(H7), C38(H38),
 C48(H48), C47(H47), C55(H55), C54(H54), C51(H51), C52(H52), C28(H28), C21(H21),
  C25(H25), C26(H26), C27(H27), C22(H22), C23(H23)
2.c Idealised Me refined as rotating group:
 C42(H42A,H42B,H42C), C56(H56A,H56B,H56C), C35(H35A,H35B,H35C), C49(H49A,H49B,
 H49C)
;
_shelx_res_checksum              61929
_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 1.376
_oxdiff_exptl_absorpt_empirical_full_min 0.783