N-Confused strapped calix[4]pyrrole: the missing member of calix[4]pyrrole chemistry.
Roy, Anik; Halder, Dibakar; Patra, Ashoke Kumar; Frontera, Antonio; Saha, Indrajit; Organic & biomolecular chemistry 22 (2024) 8249–8254; doi:10.1039/d4ob00799a

data_7160030
_publ_section_title
;
 N-Confused strapped calix[4]pyrrole: the missing member of
 calix[4]pyrrole chemistry.
;
_journal_issue                   41
_journal_name_full               'Organic &amp; biomolecular chemistry'
_journal_page_first              8249
_journal_page_last               8254
_journal_paper_doi               10.1039/d4ob00799a
_journal_volume                  22
_journal_year                    2024
_chemical_formula_moiety         'C H Cl3, C54 H65 N5 O4, H2 O'
_chemical_formula_sum            'C55 H68 Cl3 N5 O5'
_chemical_formula_weight         985.49
_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   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2024-03-04
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2024-03-15 deposited with the CCDC.	2024-07-04 downloaded from the CCDC.
;
_cell_angle_alpha                103.800(9)
_cell_angle_beta                 93.677(8)
_cell_angle_gamma                104.184(8)
_cell_formula_units_Z            2
_cell_length_a                   12.252(3)
_cell_length_b                   13.066(4)
_cell_length_c                   17.157(5)
_cell_measurement_reflns_used    7654
_cell_measurement_temperature    160.03
_cell_measurement_theta_max      25.20
_cell_measurement_theta_min      2.28
_cell_volume                     2564.0(13)
_computing_cell_refinement       'SAINT V8.38A (Bruker, 2018)'
_computing_data_reduction        'SAINT V8.38A (Bruker, 2018)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      160.03
_diffrn_detector                 'Bruker APEX2 area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker SMART APEX2 area detector'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0953
_diffrn_reflns_av_unetI/netI     0.1062
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            26193
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.149
_diffrn_reflns_theta_max         25.149
_diffrn_reflns_theta_min         2.251
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_type              'Incoatec I\ms'
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.232
_exptl_absorpt_correction_T_max  0.7080
_exptl_absorpt_correction_T_min  0.6135
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1494 before and 0.1086 after correction.
The Ratio of minimum to maximum transmission is 0.8665.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.276
_exptl_crystal_description       block
_exptl_crystal_F_000             1048
_exptl_crystal_size_max          0.8
_exptl_crystal_size_mid          0.5
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.312
_refine_diff_density_min         -0.491
_refine_diff_density_rms         0.082
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     628
_refine_ls_number_reflns         9165
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.1041
_refine_ls_R_factor_gt           0.0736
_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^)+(0.1124P)^2^+0.8482P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1861
_refine_ls_wR_factor_ref         0.2195
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6331
_reflns_number_total             9165
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4ob00799a2.cif
_cod_data_source_block           mo_ad180823_0m
_cod_depositor_comments
'Adding full bibliography for 7160030--7160031.cif.'
_cod_original_cell_volume        2564.0(12)
_cod_database_code               7160030
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.955
_shelx_estimated_absorpt_t_min   0.836
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2.a Free rotating group:
 O5(H5C,H5D)
2.b Ternary CH refined with riding coordinates:
 C55(H55)
2.c Secondary CH2 refined with riding coordinates:
 C52(H52A,H52B), C3(H3A,H3B), C41(H41A,H41B), C7(H7A,H7B), C47(H47A,H47B),
 C5(H5A,H5B)
2.d Aromatic/amide H refined with riding coordinates:
 N2(H2), N1(H1), N5(H5), N3(H3), N4(H4), C30(H30), C22(H22), C9(H9), C17(H17),
 C20(H20), C28(H28), C1(H1A), C19(H19), C49(H49), C45(H45), C51(H51), C46(H46)
2.e Idealised Me refined as rotating group:
 C38(H38A,H38B,H38C), C54(H54A,H54B,H54C), C39(H39A,H39B,H39C), C42(H42A,H42B,
 H42C), C13(H13A,H13B,H13C), C43(H43A,H43B,H43C), C35(H35A,H35B,H35C), C44(H44A,
 H44B,H44C), C36(H36A,H36B,H36C), C23(H23A,H23B,H23C), C24(H24A,H24B,H24C),
 C25(H25A,H25B,H25C)
;
_shelx_res_checksum              71342
_olex2_submission_special_instructions 'No special instructions were received'