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_7127250
_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         'C47 H31 F5 N2 O'
_chemical_formula_sum            'C47 H31 F5 N2 O'
_chemical_formula_weight         734.77
_chemical_name_systematic        'carbatriphyrin[3.1.1] fused monomer'
_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
_atom_sites_solution_primary     dual
_audit_creation_date             2018-12-10
_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                71.893(6)
_cell_angle_beta                 73.259(7)
_cell_angle_gamma                69.076(6)
_cell_formula_units_Z            2
_cell_length_a                   10.4374(7)
_cell_length_b                   13.2672(8)
_cell_length_c                   16.3284(12)
_cell_measurement_reflns_used    5174
_cell_measurement_temperature    113(20)
_cell_measurement_theta_max      73.7150
_cell_measurement_theta_min      3.6820
_cell_volume                     1967.1(3)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46b (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46b (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46b (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_environment      N~2~
_diffrn_ambient_temperature      113(20)
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            'Pilatus 200K'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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    -44.00   6.00   0.50   11.00    --    0.00 115.00  54.00  100
  2  \w     65.00 158.00   0.50   11.00    --  102.08 168.00-161.00  186
  3  \w     99.00 168.00   0.50   11.00    --  102.08 115.00  54.00  138
  4  \w     48.00 148.00   0.50   11.00    --  102.08-168.00-179.00  200
  5  \w     36.00 113.00   0.50   11.00    --  102.08-115.00 -35.00  154
  6  \w     -1.00  65.00   0.50   11.00    --    0.00  37.00-150.00  132
  7  \w     -1.00  65.00   0.50   11.00    --    0.00  37.00  30.00  132
  8  \w    -61.00  10.00   0.50   11.00    --    0.00 -57.00 -90.00  142
  9  \w     -1.00  65.00   0.50   11.00    --    0.00  37.00  90.00  132
 10  \w     40.00 114.00   0.50   11.00    --  102.08 -61.00  30.00  148
 11  \w     40.00 124.00   0.50   11.00    --  102.08 -77.00 150.00  168
 12  \w     39.00 105.00   0.50   11.00    --  102.08 -45.00  90.00  132
 13  \w     34.00 109.00   0.50   11.00    --  102.08 -94.00   0.00  150
 14  \w    100.00 165.00   0.50   11.00    --  102.08  45.00 -60.00  130
 15  \w     36.00 103.00   0.50   11.00    --  102.08 -30.00 150.00  134
 16  \w     40.00 114.00   0.50   11.00    --  102.08 -61.00 150.00  148
 17  \w    100.00 165.00   0.50   11.00    --  102.08  45.00-180.00  130
 18  \w    100.00 165.00   0.50   11.00    --  102.08  45.00 -30.00  130
 19  \w     39.00 118.00   0.50   11.00    --  102.08-125.00 -60.00  158
 20  \w     39.00 118.00   0.50   11.00    --  102.08-125.00-180.00  158
 21  \w     40.00 114.00   0.50   11.00    --  102.08 -61.00 -90.00  148
 22  \w     36.00 103.00   0.50   11.00    --  102.08 -30.00-150.00  134
 23  \w    100.00 165.00   0.50   11.00    --  102.08  45.00  30.00  130
 24  \w     36.00 103.00   0.50   11.00    --  102.08 -30.00   0.00  134
 25  \w     39.00 105.00   0.50   11.00    --  102.08 -45.00 -60.00  132
 26  \w    101.00 169.00   0.50   11.00    --  102.08  30.00 -60.00  136
 27  \w     34.00 104.00   0.50   11.00    --  102.08 -15.00 150.00  140
 28  \w     34.00 109.00   0.50   11.00    --  102.08 -94.00  60.00  150
 29  \w    100.00 170.00   0.50   11.00    --  102.08  15.00   0.00  140
 30  \w     -1.00  65.00   0.50   11.00    --    0.00  37.00 -30.00  132
 31  \w     -1.00  62.00   0.50   11.00    --    0.00  19.00 150.00  126
 32  \w     -1.00  65.00   0.50   11.00    --    0.00  37.00 -90.00  132
;
_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      0.0335364000
_diffrn_orient_matrix_UB_12      0.0020153000
_diffrn_orient_matrix_UB_13      -0.0986570000
_diffrn_orient_matrix_UB_21      0.1133298000
_diffrn_orient_matrix_UB_22      0.0567735000
_diffrn_orient_matrix_UB_23      -0.0157553000
_diffrn_orient_matrix_UB_31      0.1097098000
_diffrn_orient_matrix_UB_32      -0.1144983000
_diffrn_orient_matrix_UB_33      0.0167388000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.1887
_diffrn_reflns_av_unetI/netI     0.1535
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            28432
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         68.249
_diffrn_reflns_theta_min         3.667
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.751
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.72485
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46b (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'metallic blackish brown'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   blackish
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.240
_exptl_crystal_description       block
_exptl_crystal_F_000             760
_exptl_crystal_preparation
'The sample was prepared by diffusion of hexane into chloroform solution'
_exptl_crystal_recrystallization_method
'The sample was crystallized by vapour difussion technique'
_exptl_crystal_size_max          0.929
_exptl_crystal_size_mid          0.351
_exptl_crystal_size_min          0.269
_refine_diff_density_max         0.648
_refine_diff_density_min         -0.511
_refine_diff_density_rms         0.093
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     501
_refine_ls_number_reflns         7189
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.018
_refine_ls_R_factor_all          0.1577
_refine_ls_R_factor_gt           0.0997
_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^)+(0.1640P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2694
_refine_ls_wR_factor_ref         0.3064
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3807
_reflns_number_total             7189
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0cc05309k2.cif
_cod_data_source_block           as_23pibhy_fm
_cod_depositor_comments
;
Adding full bibliography for 7127249--7127250.cif.

2025-03-04
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C3.36 H2.21 F0.36 N0.14 O0.07'
_cod_original_formula_weight         52.48
_cod_original_formula_moiety         '0.07(C47 H31 F5 N2 O)'
_cod_original_formula_units_Z            28
_cod_database_code               7127250
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         'C H N F O'
_diffrn_oxdiff_ac3_digest_frames
;
014922cd906226a37e1823ac22b64675270002588f9
;
_diffrn_oxdiff_ac3_digest_hkl
;
01dd8589037a9ac05739150ae9606d85076d0c
;
_reflns_odcompleteness_completeness 99.96
_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. Uiso/Uaniso restraints and constraints
F3 \\sim F4 \\sim F5: within 2A with sigma of 0.04 and sigma for terminal atoms
of 0.08
3.a Aromatic/amide H refined with riding coordinates:
 N2(H2), C1"(H1"), C1'(H1'), C2"(H2"), C2'(H2'), C5(H5), C6(H6), C15(H15),
 C16(H16), C17(H17), C19(H19), C20(H20), C21(H21), C23(H23), C29(H29), C31(H31)
3.b Idealised Me refined as rotating group:
 C25(H25A,H25B,H25C), C26(H26A,H26B,H26C), C33(H33A,H33B,H33C), C34(H34A,H34B,
 H34C), C35(H35A,H35B,H35C)
;
_shelx_res_checksum              13945
_shelx_fab_checksum              69345
_olex2_exptl_crystal_mounting_method
'The crystal was mounted by means of paratonic oil'
_olex2_submission_original_sample_id 'carbatriphyrin[3.1.1] fused monomer'
_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 3.279
_oxdiff_exptl_absorpt_empirical_full_min 0.309