Calixarene alpha-ketoacetylenes: versatile platforms for reaction with hydrazine nucleophile
Muravev, Anton A.; Solovieva, Svetlana E.; Galieva, Farida B.; Bazanova, Olga B.; Rizvanov, Ildar Kh.; Ivshin, Kamil A.; Kataeva, Olga N.; Matthews, Susan E.; Antipin, Igor S.; RSC Advances 8 (2018) 32765–; doi:10.1039/C8RA06349D

data_7231551
_publ_section_title
;
 Calixarene alpha-ketoacetylenes: versatile platforms for reaction with
 hydrazine nucleophile
;
_journal_issue                   57
_journal_name_full               'RSC Advances'
_journal_page_first              32765
_journal_paper_doi               10.1039/C8RA06349D
_journal_volume                  8
_journal_year                    2018
_chemical_formula_moiety         'C84 H80 O8'
_chemical_formula_sum            'C84 H80 O8'
_chemical_formula_weight         1217.48
_space_group_crystal_system      tetragonal
_space_group_IT_number           88
_space_group_name_Hall           '-I 4ad'
_space_group_name_H-M_alt        'I 41/a'
_symmetry_space_group_name_Hall  '-I 4ad'
_symmetry_space_group_name_H-M   'I 41/a :2'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2017-10-10 deposited with the CCDC.
2018-09-17 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.0450(4)
_cell_length_b                   13.0450(4)
_cell_length_c                   40.2669(12)
_cell_measurement_reflns_used    9928
_cell_measurement_temperature    198(2)
_cell_measurement_theta_max      65.04
_cell_measurement_theta_min      3.56
_cell_volume                     6852.3(4)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'MERCURY 3.7 (Macrae, 2015)'
_computing_publication_material  'enCIFer 1.5.1 (Allen et al. 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      198(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Bruker Kappa APEX DUO CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0225
_diffrn_reflns_av_unetI/netI     0.0205
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       47
_diffrn_reflns_limit_l_min       -47
_diffrn_reflns_number            17469
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         68.257
_diffrn_reflns_theta_min         3.561
_diffrn_source                   'microfocus X-Ray tube'
_exptl_absorpt_coefficient_mu    0.586
_exptl_absorpt_correction_T_max  0.4774
_exptl_absorpt_correction_T_min  0.2665
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS version 2.10 (Sheldrick,Bruker AXS Inc.)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.180
_exptl_crystal_description       prizm
_exptl_crystal_F_000             2592
_exptl_crystal_size_max          0.724
_exptl_crystal_size_mid          0.300
_exptl_crystal_size_min          0.208
_refine_diff_density_max         0.222
_refine_diff_density_min         -0.285
_refine_diff_density_rms         0.076
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     211
_refine_ls_number_reflns         3122
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0479
_refine_ls_R_factor_gt           0.0462
_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^)+(0.0733P)^2^+2.9429P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1272
_refine_ls_wR_factor_ref         0.1288
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2917
_reflns_number_total             3122
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8ra06349d2.cif
_cod_data_source_block           an255-abs_a
_cod_original_cell_volume        6852.3(5)
_cod_database_code               7231551
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.676
_shelx_estimated_absorpt_t_max   0.888
_shelx_res_checksum              14209