Pyrrolizinofluorene-embedded dithiacalixcorrole(1.0.<i>1</i>.<i>1</i>)s.
Varak, Pooja; Ravikanth, Mangalampalli; Organic & biomolecular chemistry 22 (2024) 8125–8132; doi:10.1039/d4ob01276c

data_7160143
_publ_section_title
;
 Pyrrolizinofluorene-embedded dithiacalixcorrole(1.0.<i>1</i>.<i>1</i>)s.
;
_journal_issue                   40
_journal_name_full               'Organic &amp; biomolecular chemistry'
_journal_page_first              8125
_journal_page_last               8132
_journal_paper_doi               10.1039/d4ob01276c
_journal_volume                  22
_journal_year                    2024
_chemical_formula_moiety         'C57 H40 N2 O2 S3'
_chemical_formula_sum            'C57 H40 N2 O2 S3'
_chemical_formula_weight         881.09
_chemical_name_common            Calixcorrole
_chemical_name_systematic
'Pyrrolizinofluorene-Embedded Dithiacalixcorrole'
_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
_audit_creation_date             2024-06-25
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2024-06-25 deposited with the CCDC.	2024-09-13 downloaded from the CCDC.
;
_cell_angle_alpha                100.139(5)
_cell_angle_beta                 90.991(6)
_cell_angle_gamma                94.836(5)
_cell_formula_units_Z            2
_cell_length_a                   11.9857(9)
_cell_length_b                   13.2787(8)
_cell_length_c                   13.8288(10)
_cell_measurement_reflns_used    4299
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      24.0940
_cell_measurement_theta_min      1.9790
_cell_volume                     2157.7(3)
_computing_cell_refinement       'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      150.15
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \f    -10.27 349.73   2.00   10.00  72.69 -18.16  31.50    --   180
  2  \w    -76.17   5.83   2.00   10.00    --  -18.16  89.85  18.34   41
  3  \w    -76.17   5.83   2.00   10.00    --  -18.16  89.85-137.66   41
  4  \w   -122.88  23.12   2.00   10.00    --  -18.16 -59.25-135.92   73
  5  \w    -76.17   5.83   2.00   10.00    --  -18.16  89.85 171.34   41
  6  \w   -122.88  23.12   2.00   10.00    --  -18.16 -59.25  71.08   73
  7  \f   -349.73  10.27   2.00   10.00  31.11 -18.16 -31.50    --   180
  8  \w    -76.17   5.83   2.00   10.00    --  -18.16  89.85  69.33   41
  9  \w    -76.17   5.83   2.00   10.00    --  -18.16  89.85 -32.66   41
 10  \w   -122.88  23.12   2.00   10.00    --  -18.16 -59.25 -84.92   73
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type
'Saxi-CrysAlisPro-abstract goniometer imported SAXI images'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1502
_diffrn_reflns_av_unetI/netI     0.0854
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            61621
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         1.564
_exptl_absorpt_coefficient_mu    0.221
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.50352
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.49 (Rigaku Oxford Diffraction, 2022)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            Brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.356
_exptl_crystal_description       block
_exptl_crystal_F_000             920
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.089
_refine_diff_density_max         1.361
_refine_diff_density_min         -0.473
_refine_diff_density_rms         0.089
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     579
_refine_ls_number_reflns         7602
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.1239
_refine_ls_R_factor_gt           0.0816
_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^)+(0.1221P)^2^+3.1222P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2117
_refine_ls_wR_factor_ref         0.2464
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4906
_reflns_number_total             7602
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4ob01276c2.cif
_cod_data_source_block           mr_pv_flu_autored
_cod_depositor_comments          'Adding full bibliography for 7160143.cif.'
_cod_database_code               7160143
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.981
_shelx_estimated_absorpt_t_min   0.957
_olex2_refinement_description
;
1.a Ternary CH refined with riding coordinates:
 C33(H33), C8(H8), C28(H28)
1.b Aromatic/amide H refined with riding coordinates:
 N2(H2), C6(H6), C1(H1), C2(H2A), C16(H16), C45(H45), C50(H50), C49(H49),
 C46(H46), C35(H35), C22(H22), C13(H13), C21(H21), C31(H31), C10(H10), C41(H41),
  C12(H12), C25(H25), C30(H30), C26(H26), C57(H57), C11(H11), C43(H43),
 C56(H56), C52(H52), C53(H53), C39(H39), C42(H42), C36(H36), C37(H37), C40(H40)
1.c Idealised Me refined as rotating group:
 C48(H48A,H48B,H48C), C55(H55A,H55B,H55C)
;
_shelx_res_checksum              69650
_shelx_hkl_checksum              41526
_shelx_fab_checksum              93941
_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
;