De novo fabrication of higher arene ring incorporated contorted calix[2]phyrin(2.2.1.1.1) and its F− bound complex
Pradhan, Sourav Ranjan; Prasad, Chetan Kumar; Das, Mainak; Srinivasan, A.; Dalton Transactions 53 (2024) 15258–15263; doi:10.1039/D4DT01903B

data_7717152
_publ_section_title
;
 De novo fabrication of higher arene ring incorporated contorted
 calix[2]phyrin(2.2.1.1.1) and its F&#x2212; bound complex
;
_journal_issue                   36
_journal_name_full               'Dalton Transactions'
_journal_page_first              15258
_journal_page_last               15263
_journal_paper_doi               10.1039/D4DT01903B
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety         'C45 H40 N2'
_chemical_formula_sum            'C45 H40 N2'
_chemical_formula_weight         608.79
_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     dual
_audit_creation_date             2024-04-21
_audit_creation_method
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_audit_update_record
;
2024-04-22 deposited with the CCDC.	2024-08-20 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 95.6400(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.0411(2)
_cell_length_b                   25.9133(3)
_cell_length_c                   7.63460(10)
_cell_measurement_reflns_used    18951
_cell_measurement_temperature    111.5(10)
_cell_measurement_theta_max      76.3430
_cell_measurement_theta_min      4.9000
_cell_volume                     3551.93(7)
_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 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2014/7 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      111.5(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            'Pilatus 200K'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.968
_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    -22.00  62.00   0.50    4.00    --    0.00  77.00 -14.00  168
  2  \w    -62.00  22.00   0.50    4.00    --    0.00 -77.00-140.00  168
  3  \w     80.00 164.00   0.50   16.00    --  102.08  77.00 -14.00  168
  4  \w     40.00 124.00   0.50   16.00    --  102.08 -77.00-140.00  168
  5  \w     -1.00  65.00   0.50    4.00    --    0.00  37.00 150.00  132
  6  \w     -1.00  65.00   0.50    4.00    --    0.00  37.00-120.00  132
  7  \w     36.00 103.00   0.50   16.00    --  102.08 -30.00-120.00  134
  8  \w     36.00 103.00   0.50   16.00    --  102.08 -30.00 -30.00  134
  9  \w    100.00 165.00   0.50   16.00    --  102.08  45.00-180.00  130
 10  \w     34.00 104.00   0.50   16.00    --  102.08 -15.00-120.00  140
 11  \w     36.00 103.00   0.50   16.00    --  102.08 -30.00-180.00  134
 12  \w     34.00 104.00   0.50   16.00    --  102.08 -15.00  30.00  140
 13  \w     40.00 114.00   0.50   16.00    --  102.08 -61.00  90.00  148
 14  \w     94.00 166.00   0.50   16.00    --  102.08 125.00 -90.00  144
 15  \w    100.00 165.00   0.50   16.00    --  102.08  45.00 -90.00  130
 16  \w    -10.00  61.00   0.50    4.00    --    0.00  57.00  60.00  142
 17  \w    -62.00  -9.00   0.50    4.00    --    0.00 -77.00  30.00  106
 18  \w     -1.00  67.00   0.50    4.00    --    0.00  19.00 -30.00  136
;
_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      -0.0809233000
_diffrn_orient_matrix_UB_12      0.0111628000
_diffrn_orient_matrix_UB_13      0.0368063000
_diffrn_orient_matrix_UB_21      -0.0261844000
_diffrn_orient_matrix_UB_22      -0.0484291000
_diffrn_orient_matrix_UB_23      -0.1054026000
_diffrn_orient_matrix_UB_31      0.0113698000
_diffrn_orient_matrix_UB_32      -0.0326228000
_diffrn_orient_matrix_UB_33      0.1692546000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0546
_diffrn_reflns_av_unetI/netI     0.0307
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.968
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            26987
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.968
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         77.017
_diffrn_reflns_theta_min         3.411
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.497
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.58860
_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 light yellow'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.138
_exptl_crystal_description       block
_exptl_crystal_F_000             1296
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.218
_refine_diff_density_min         -0.290
_refine_diff_density_rms         0.050
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.103
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     426
_refine_ls_number_reflns         7285
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.103
_refine_ls_R_factor_all          0.0601
_refine_ls_R_factor_gt           0.0544
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0958P)^2^+0.6341P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1533
_refine_ls_wR_factor_ref         0.1575
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6336
_reflns_number_total             7285
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt01903b2.cif
_cod_data_source_block           vc-sn-cal-pyr
_cod_database_code               7717152
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'C180 H160 N8 '
_shelx_estimated_absorpt_t_max   0.952
_shelx_estimated_absorpt_t_min   0.907
_olex2_refinement_description
;
1.a Ternary CH refined with riding coordinates:
 C18(H18), C8(H8)
1.b Secondary CH2 refined with riding coordinates:
 C37(H37A,H37B), C38(H38A,H38B)
1.c Aromatic/amide H refined with riding coordinates:
 N2(H2), N1(H1), C28(H28), C45(H45), C29(H29), C3(H3), C20(H20), C11(H11),
 C26(H26), C23(H23), C27(H27), C41(H41), C4(H4), C10(H10), C6(H6), C22(H22),
 C5(H5), C44(H44), C21(H21), C16(H16), C43(H43), C15(H15), C42(H42), C35(H35),
 C31(H31), C34(H34), C33(H33), C32(H32)
1.d Idealised Me refined as rotating group:
 C36(H36A,H36B,H36C), C39(H39A,H39B,H39C)
;
_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 3.445
_oxdiff_exptl_absorpt_empirical_full_min 0.147