Targeted synthesis of a positional isomer of aromatic <i>N</i>-methyl <i>N</i>-confused corrole and its organocopper(III) complex.
Panua, Anirban; Velmurugan, Gunasekaran; Comba, Peter; Rath, Harapriya; Chemical communications (Cambridge, England) 61 (2025) 17436–17439; doi:10.1039/d5cc05372b

data_7135056
_publ_section_title
;
 Targeted synthesis of a positional isomer of aromatic <i>N</i>-methyl
 <i>N</i>-confused corrole and its organocopper(III) complex.
;
_journal_issue                   89
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              17436
_journal_page_last               17439
_journal_paper_doi               10.1039/d5cc05372b
_journal_volume                  61
_journal_year                    2025
_chemical_formula_moiety         C38H22F6N4
_chemical_formula_sum            'C38 H22 F6 N4'
_chemical_formula_weight         648.59
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     'Intrinsic Phasing'
_audit_creation_method
;FinalCif 2024.9-RC113 by Daniel Kratzert, Freiburg 2025, 
https://linkprotect.cudasvc.com/url?a=https%3a%2f%2fdkratzert.de%2ffinalcif.html&c=E,1,G1AUeGViLTfS6NdVNpsDi2uPAxtfZEFER17o-SgyucZYEtTy7-9IpH61SUKFLr4kzRTP5zovkI90DK8-VMnL-gSDDQCtKDYbHwFL4IVvQ3p5xQ,,&typo=1
;
_audit_update_record
;
2025-06-24 deposited with the CCDC.	2025-10-06 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 112.310(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.100(3)
_cell_length_b                   17.498(3)
_cell_length_c                   13.593(3)
_cell_measurement_reflns_used    4925
_cell_measurement_temperature    152(2)
_cell_measurement_theta_max      19.5734
_cell_measurement_theta_min      2.575
_cell_measurement_wavelength     0.71073
_cell_volume                     3762.8(12)
_computing_cell_refinement       'SAINT V8.41 (Bruker AXS LLC)'
_computing_data_reduction        'SAINT V8.41 (Bruker AXS LLC)'
_computing_molecular_graphics    'shelXle (C.B. Huebschle, rev 1503)'
_computing_structure_refinement  'SHELXL-2019/2 (Sheldrick, 2019)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      152(2)
_diffrn_detector                 CPAD
_diffrn_detector_area_resol_mean 7.391
_diffrn_detector_type            'Bruker PHOTON III'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_details
;<Phi   scan: start= 360.0; len= 180.0; end= 540.0 at [Counterclockwise Eulerian 
angles: dx= 50.00 mm theta=   0.000 deg omega= 360.000 deg chi=  54.740 deg] 
measure for 1.0 seconds; frame angle 1.00 degrees, wavelength=0.71073>
<Phi   scan: start= 180.0; len= 180.0; end= 360.0 at [Counterclockwise Eulerian 
angles: dx= 50.00 mm theta=   0.000 deg omega= 360.000 deg chi=  54.740 deg] 
measure for 1.0 seconds; frame angle 1.00 degrees, wavelength=0.71073>
<Phi   scan: start= 360.0; len=   1.0; end= 361.0 at [Counterclockwise Eulerian 
angles: dx= 50.00 mm theta=   5.249 deg omega= 269.360 deg chi=  24.000 deg] 
measure for 2.0 seconds; frame angle 1.00 degrees, wavelength=0.71073>
<Omega scan: start=   2.5; len= 122.0; end= 124.5 at [Counterclockwise Eulerian 
angles: dx= 50.00 mm theta=   5.249 deg phi= 360.000 deg chi= -44.500 deg] 
measure for 2.0 seconds; frame angle 1.00 degrees, wavelength=0.71073>
<Omega scan: start=   2.5; len= 122.0; end= 124.5 at [Counterclockwise Eulerian 
angles: dx= 50.00 mm theta=   5.249 deg phi= 144.000 deg chi= -44.500 deg] 
measure for 2.0 seconds; frame angle 1.00 degrees, wavelength=0.71073>
<Phi   scan: start= 360.0; len=   1.0; end= 361.0 at [Counterclockwise Eulerian 
angles: dx= 50.00 mm theta=   5.249 deg omega=   1.491 deg chi= -44.500 deg] 
measure for 2.0 seconds; frame angle 1.00 degrees, wavelength=0.71073>
;
_diffrn_measurement_device       'KAPPA diffractometer'
_diffrn_measurement_device_type  'Bruker D8 VENTURE'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_measurement_specimen_support 'nylon loop'
_diffrn_radiation_monochromator  'multilayer mirror'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.2405
_diffrn_reflns_av_unetI/netI     0.0890
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            97839
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_reduction_process narrow-frame
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.0
_diffrn_reflns_theta_min         1.994
_diffrn_source                   'microfocus sealed tube'
_diffrn_source_current           1.1
_diffrn_source_target            Mo
_diffrn_source_type              'INCOATEC I\mS 3.0'
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    0.089
_exptl_absorpt_correction_T_max  0.993
_exptl_absorpt_correction_T_min  0.984
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;Krause, L., Herbst-Irmer, R., Sheldrick, G. M., Stalke, D. (2015).
"Comparison of silver and molybdenum microfocus X-ray sources for single-crystal
 structure determination"
J. Appl. Cryst. 48, 3-10.
doi:10.1107/S1600576714022985
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.145
_exptl_crystal_description       block
_exptl_crystal_F_000             1328
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.711
_refine_diff_density_min         -0.335
_refine_diff_density_rms         0.080
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.102
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     434
_refine_ls_number_reflns         6634
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.106
_refine_ls_R_factor_all          0.1813
_refine_ls_R_factor_gt           0.1217
_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^)+(0.1268P)^2^+10.9027P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2939
_refine_ls_wR_factor_ref         0.3316
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3809
_reflns_number_total             6634
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5cc05372b2.cif
_cod_data_source_block           mo_hr_ap_19052025_a_sq
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_exptl_absorpt_correction_type' value 'Multi-Scan' was
changed to 'multi-scan' in accordance with the
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 8170 2020-07-09 18:12:32Z antanas 

 Adding full bibliography for 7135056.cif.
;
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7135056
_shelx_shelxl_version_number     2019/3
_exptl_bruker_absorpt_correction_t_ratio 0.8816
_shelx_estimated_absorpt_t_min   0.984
_shelx_estimated_absorpt_t_max   0.993
_bruker_diffrn_measurement_temperature_device 'Oxford Cryostream 1000'
_diffrn_measurement_bruker_total_exposure_time 2288.0
_diffrn_reflns_bruker_av_norm_i  296.711
_diffrn_reflns_bruker_number_gt  22154
_computing_bruker_data_scaling
'SADABS-2016/2 - Bruker AXS area detector scaling and absorption correction'
_geom_details
; All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
_shelx_res_checksum              30410
_shelx_hkl_checksum              30039
_shelx_fab_checksum              46559