Triazolated calix[4]arenes from 2-azidoethylated precursors: is there a difference in the way the triazoles are attached to narrow rims?
Gorbunov, Alexander; Kuznetsova, Julia; Puchnin, Kirill; Kovalev, Vladimir; Vatsouro, Ivan; New Journal of Chemistry 43 (2019) 4562–; doi:10.1039/C8NJ06464D

data_7058184
_publ_section_title
;
 Triazolated calix[4]arenes from 2-azidoethylated precursors: is there a
 difference in the way the triazoles are attached to narrow rims?
;
_journal_issue                   11
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              4562
_journal_paper_doi               10.1039/C8NJ06464D
_journal_volume                  43
_journal_year                    2019
_chemical_formula_moiety         'C78 H90 N6 O4'
_chemical_formula_sum            'C78 H90 N6 O4'
_chemical_formula_weight         1175.55
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2018-11-25
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2018-11-25 deposited with the CCDC.    2019-02-19 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 94.043(8)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.564(2)
_cell_length_b                   22.418(4)
_cell_length_c                   22.576(3)
_cell_measurement_reflns_used    9903
_cell_measurement_temperature    120
_cell_measurement_theta_max      73.87
_cell_measurement_theta_min      2.78
_cell_volume                     6847.8(18)
_computing_cell_refinement       'APEX3 v.2017.3_0 (Bruker AXS, 2017)'
_computing_data_collection       'APEX3 v.2017.3_0 (Bruker AXS, 2017)'
_computing_data_reduction        'SAINT v8.38A (Bruker AXS, 2016)'
_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_temperature      120
_diffrn_detector                 'Bruker PHOTON 100 CMOS'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CMOS sensor'
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device       '3-circle diffractometer'
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'focusing mirrors'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0584
_diffrn_reflns_av_unetI/netI     0.0638
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            42315
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        66.596
_diffrn_reflns_theta_max         66.596
_diffrn_reflns_theta_min         2.781
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\mS microsource'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.545
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.9285
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0612 before and 0.0504 after correction. The Ratio of minimum to maximum transmission is 0.9285. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.140
_exptl_crystal_description       block
_exptl_crystal_F_000             2528
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: CHCl3, Ethanol'
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.561
_refine_diff_density_min         -0.562
_refine_diff_density_rms         0.055
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     816
_refine_ls_number_reflns         11952
_refine_ls_number_restraints     17
_refine_ls_restrained_S_all      1.077
_refine_ls_R_factor_all          0.0951
_refine_ls_R_factor_gt           0.0539
_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^)+(0.0801P)^2^+1.1678P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1370
_refine_ls_wR_factor_ref         0.1650
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7528
_reflns_number_total             11952
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8nj06464d2.cif
_cod_data_source_block           ky71
_cod_depositor_comments
;
The following automatic conversions were performed:

'_diffrn_radiation_probe' value 'X-ray' changed to 'x-ray' according
to
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 4973 2017-02-22 13:04:09Z antanas 

 Adding full bibliography for 7058184.cif.
;
_cod_original_cell_volume        6847.4(18)
_cod_database_code               7058184
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.943
_shelx_estimated_absorpt_t_min   0.928
_computing.bruker_data_scaling   'SADABS V2012/1 (Bruker AXS Inc.)'
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C49-C51 = C49-C50
 1.54 with sigma of 0.01
 C38-C37 \\sim C39-C37 \\sim C40-C37 \\sim C41-C37 \\sim C42-C37 \\sim C43-C37
 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
Uanis(C51) = Uanis(C49) = Uanis(C50)
Uanis(C41) = Uanis(C40)
Uanis(C39) = Uanis(C38)
Uanis(C42) = Uanis(C43)
4. Others
 Fixed Sof: C40(0.33333) H40A(0.33333) H40B(0.33333) H40C(0.33333)
 C42(0.33333) H42A(0.33333) H42B(0.33333) H42C(0.33333) C39(0.66667)
 H39A(0.66667) H39B(0.66667) H39C(0.66667) C50(0.8) H50A(0.8) H50B(0.8)
 H50C(0.8) C51(0.2) H51A(0.2) H51B(0.2) H51C(0.2) C43(0.66667) H43A(0.66667)
 H43B(0.66667) H43C(0.66667) C41(0.66667) H41A(0.66667) H41B(0.66667)
 H41C(0.66667) C38(0.33333) H38A(0.33333) H38B(0.33333) H38C(0.33333) H49A(0.8)
 H49B(0.8) H49C(0.2) H49D(0.2)
5.a Riding coordinates:
 C30(H30A,H30B,H30C)
5.b Secondary CH2 refined with riding coordinates:
 C16(H16A,H16B), C12(H12A,H12B), C4(H4A,H4B), C69(H69A,H69B), C55(H55A,H55B),
 C8(H8A,H8B), C56(H56A,H56B), C70(H70A,H70B), C52(H52A,H52B), C48(H48A,H48B),
 C53(H53A,H53B), C49(H49A,H49B), C49(H49C,H49D)
5.c Aromatic/amide H refined with riding coordinates:
 C17(H17), C26(H26), C57(H57), C20(H20), C19(H19), C68(H68), C67(H67),
 C28(H28), C23(H23), C60(H60), C25(H25), C22(H22), C62(H62), C63(H63), C71(H71),
  C65(H65), C74(H74), C64(H64), C82(H82), C81(H81), C79(H79), C76(H76),
 C78(H78), C77(H77)
5.d Idealised Me refined as rotating group:
 C45(H45A,H45B,H45C), C46(H46A,H46B,H46C), C34(H34A,H34B,H34C), C47(H47A,H47B,
 H47C), C35(H35A,H35B,H35C), C36(H36A,H36B,H36C), C31(H31A,H31B,H31C), C32(H32A,
 H32B,H32C), C54(H54A,H54B,H54C), C40(H40A,H40B,H40C), C42(H42A,H42B,H42C),
 C39(H39A,H39B,H39C), C50(H50A,H50B,H50C), C51(H51A,H51B,H51C), C43(H43A,H43B,
 H43C), C41(H41A,H41B,H41C), C38(H38A,H38B,H38C)
;
_shelx_res_checksum              40937
_olex2_submission_special_instructions 'No special instructions were received'