PtCl<sub>2</sub> mediated peripheral transformation of carbatriphyrin(3.1.1) into a <i>meso</i>-fused β-β' dimer and its monomer analogue.
Murugavel, M.; Adinarayana, B.; Das, Mainak; Peruncheralathan, S.; Palepu, Narasinga Rao; Srinivasan, A.; Chemical communications (Cambridge, England) 56 (2020) 12809–12812; doi:10.1039/d0cc05309k

data_7127249
_publ_section_title
;
 PtCl<sub>2</sub> mediated peripheral transformation of
 carbatriphyrin(3.1.1) into a <i>meso</i>-fused \b-\b' dimer and its
 monomer analogue.
;
_journal_issue                   84
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              12809
_journal_page_last               12812
_journal_paper_doi               10.1039/d0cc05309k
_journal_volume                  56
_journal_year                    2020
_chemical_formula_moiety         'C94 H64 F10 N4'
_chemical_formula_sum            'C94 H64 F10 N4'
_chemical_formula_weight         1439.49
_chemical_name_systematic        'carbatriphyrin fused dimer'
_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     dual
_audit_creation_date             2018-08-08
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5337)
;
_audit_update_record
;
2019-09-19 deposited with the CCDC.	2020-09-14 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90.863(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   24.2592(6)
_cell_length_b                   14.9349(6)
_cell_length_c                   21.0144(5)
_cell_measurement_reflns_used    14750
_cell_measurement_temperature    100
_cell_measurement_theta_max      76.1040
_cell_measurement_theta_min      3.4620
_cell_volume                     7612.8(4)
_computing_cell_refinement       'CrysAlisPro 1.171.39.29d (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.29d (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.29d (Rigaku OD, 2017)'
_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      100
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            'Pilatus 200K'
_diffrn_measured_fraction_theta_full 0.997
_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    -94.00  -8.00   0.50    2.44    --  -38.50 134.00  55.00  172
  2  \w    -95.00  -8.00   0.50    2.44    --  -38.50 135.00-125.00  174
  3  \w     30.00 105.00   0.50    2.44    --   49.06-134.00 -12.00  150
  4  \w     29.00 106.00   0.50    2.44    --   49.06-135.00 168.00  154
  5  \w     43.00 126.00   0.50    8.80    --  106.38-135.00 168.00  166
  6  \w     89.00 170.00   0.50    8.80    --  106.38 134.00  55.00  162
  7  \w     89.00 169.00   0.50    8.80    --  106.38 135.00-125.00  160
  8  \w     64.00 124.00   0.50    8.80    --  106.38-134.00 -12.00  120
  9  \w    -41.00  27.00   0.50    2.44    --  -38.50  37.00 150.00  136
 10  \w    -60.00 -27.00   0.50    2.44    --  -38.50 -57.00   0.00   66
 11  \w   -101.00 -67.00   0.50    2.44    --  -38.50 -57.00   0.00   68
 12  \w     79.00 110.00   0.50    2.44    --   49.06  57.00-120.00   62
 13  \w     38.00  69.00   0.50    2.44    --   49.06  57.00-120.00   62
 14  \w     93.00 119.00   0.50    8.80    --  106.38  77.00 120.00   52
 15  \w     44.00 120.00   0.50    8.80    --  106.38 -61.00 120.00  152
 16  \w    113.00 169.00   0.50    8.80    --  106.38  45.00-120.00  112
 17  \w    138.00 164.00   0.50    8.80    --  106.38  45.00-150.00   52
 18  \w    107.00 134.00   0.50    8.80    --  106.38  45.00-150.00   54
 19  \w     94.00 171.00   0.50    8.80    --  106.38 125.00  90.00  154
 20  \w     87.00 121.00   0.50    8.80    --  106.38-125.00-150.00   68
 21  \w     44.00 111.00   0.50    8.80    --  106.38 -45.00 120.00  134
 22  \w    135.00 166.00   0.50    8.80    --  106.38  77.00 120.00   62
 23  \w    103.00 164.00   0.50    8.80    --  106.38  61.00 -30.00  122
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type
'SuperNova, Dual, Cu at home/near, Pilatus 200K'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0228600000
_diffrn_orient_matrix_UB_12      -0.0961800000
_diffrn_orient_matrix_UB_13      0.0041373000
_diffrn_orient_matrix_UB_21      -0.0584911000
_diffrn_orient_matrix_UB_22      -0.0373094000
_diffrn_orient_matrix_UB_23      -0.0112409000
_diffrn_orient_matrix_UB_31      0.0093884000
_diffrn_orient_matrix_UB_32      0.0003623000
_diffrn_orient_matrix_UB_33      -0.0723506000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0885
_diffrn_reflns_av_unetI/netI     0.0567
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            27832
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         68.251
_diffrn_reflns_theta_min         3.475
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.744
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.43739
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.29d (Rigaku Oxford Diffraction, 2017)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'metallic pinkish pink'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   pinkish
_exptl_crystal_colour_primary    pink
_exptl_crystal_density_diffrn    1.256
_exptl_crystal_description       hexagonal
_exptl_crystal_F_000             2984
_exptl_crystal_recrystallization_method 'Vapour deposition'
_exptl_crystal_size_max          0.384
_exptl_crystal_size_mid          0.263
_exptl_crystal_size_min          0.21
_refine_diff_density_max         0.660
_refine_diff_density_min         -0.443
_refine_diff_density_rms         0.098
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     492
_refine_ls_number_reflns         6937
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.0998
_refine_ls_R_factor_gt           0.0900
_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^)+(0.1370P)^2^+26.5970P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2422
_refine_ls_wR_factor_ref         0.2506
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5860
_reflns_number_total             6937
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0cc05309k2.cif
_cod_data_source_block           as_mm_ptr
_cod_depositor_comments
'Adding full bibliography for 7127249--7127250.cif.'
_cod_database_code               7127249
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         'C94 H72 F10 N4'
_diffrn_oxdiff_ac3_digest_frames
;
010f140e788d4f978f55bd6616495398b20002916b4
;
_diffrn_oxdiff_ac3_digest_hkl
;
01df7ff3e7324dfd594b6e290d05af7f99d8a5
;
_reflns_odcompleteness_completeness 99.68
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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), N1(H1), C5(H5), C6(H6), C20(H20), C19(H19), C15(H15), C16(H16),
 C29(H29), C17(H17), C1'(H1'), C21(H21), C1"(H1"), C31(H31), C2'(H2'), C23(H23),
  C2"(H2")
2.b Idealised Me refined as rotating group:
 C34(H34A,H34B,H34C), C33(H33A,H33B,H33C), C35(H35A,H35B,H35C), C26(H26A,H26B,
 H26C), C25(H25A,H25B,H25C)
;
_shelx_res_checksum              81583
_shelx_fab_checksum              38146
_olex2_submission_original_sample_id 2,3-biph-FD
_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 3.489
_oxdiff_exptl_absorpt_empirical_full_min 0.192