Synthesis of a tube-like tetra-bipyridyl, tetra-ethylacetato-calix[4]arene in 1,3-alternate conformation and the unexpected crystal structure of its [bpy(CoCl2)]3-[bpy(CoCl2)(H2O)] complex
Mourer, Maxime; Bouizi, Younes; Leclerc, Sébastien; Malaman, Bernard; Regnouf de Vains, Jean-Bernard; New Journal of Chemistry 48 (2024) 15577–15589; doi:10.1039/D4NJ02476A

data_7063396
_publ_section_title
;
 Synthesis of a tube-like tetra-bipyridyl,
 tetra-ethylacetato-calix[4]arene in 1,3-alternate conformation and the
 unexpected crystal structure of its [bpy(CoCl2)]3-[bpy(CoCl2)(H2O)]
 complex
;
_journal_issue                   35
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              15577
_journal_page_last               15589
_journal_paper_doi               10.1039/D4NJ02476A
_journal_volume                  48
_journal_year                    2024
_chemical_formula_moiety         'C92 H88 Cl8 Co4 N8 O13'
_chemical_formula_sum            'C92 H88 Cl8 Co4 N8 O13'
_chemical_formula_weight         2033.1
_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_method           SHELXL-2018/3
_audit_update_record
;
2024-05-24 deposited with the CCDC.	2024-07-25 downloaded from the CCDC.
;
_cell_angle_alpha                75.598(4)
_cell_angle_beta                 83.619(5)
_cell_angle_gamma                71.724(4)
_cell_formula_units_Z            2
_cell_length_a                   13.1367(19)
_cell_length_b                   16.011(2)
_cell_length_c                   23.770(4)
_cell_measurement_reflns_used    7572
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      19
_cell_measurement_theta_min      0.9
_cell_volume                     4595.2(12)
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    olex2-1.3
_diffrn_ambient_temperature      90(2)
_diffrn_measured_fraction_theta_full 0.979
_diffrn_measured_fraction_theta_max 0.979
_diffrn_measurement_device_type  'BRUKER APEX II QUAZAR CCD'
_diffrn_measurement_method       'f\ and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0852
_diffrn_reflns_av_unetI/netI     0.0657
_diffrn_reflns_Laue_measured_fraction_full 0.979
_diffrn_reflns_Laue_measured_fraction_max 0.979
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            34764
_diffrn_reflns_point_group_measured_fraction_full 0.979
_diffrn_reflns_point_group_measured_fraction_max 0.979
_diffrn_reflns_theta_full        24
_diffrn_reflns_theta_max         24
_diffrn_reflns_theta_min         1.457
_diffrn_source                   ImuS
_exptl_absorpt_coefficient_mu    1.008
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (BRUKER, 2004)'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.469
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       parallelepiped
_exptl_crystal_F_000             2088
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: CH2Cl2 and CH3CN'
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_exptl_transmission_factor_max   0.74
_exptl_transmission_factor_min   0.48
_refine_diff_density_max         0.410
_refine_diff_density_min         -0.303
_refine_diff_density_rms         0.060
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.069
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1109
_refine_ls_number_reflns         7572
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.069
_refine_ls_R_factor_all          0.0619
_refine_ls_R_factor_gt           0.0407
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0344P)^2^+2.5892P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0839
_refine_ls_wR_factor_ref         0.0904
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5930
_reflns_number_total             7572
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4nj02476a2.cif
_cod_data_source_block           shelx
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_exptl_crystal_density_meas' value 'not measured' was
changed to '?' -- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 8170 2020-07-09 18:12:32Z antanas 

 Adding full bibliography for 7063396.cif.
;
_cod_database_code               7063396
_shelx_shelxl_version_number     2018/3
_shelx_res_checksum              6254
_shelx_hkl_checksum              68884