Revealing the remarkable structural diversity of the alkali metal transfer agents of the trans-calix[2]benzene[2]pyrrolide ligand.
Fuentes, M Ángeles; Martínez-Martínez, Antonio J; Kennedy, Alan R.; Mulvey, Robert E.; Chemical communications (Cambridge, England) 52 (2016) 12199–12201; doi:10.1039/c6cc07240b

data_7125160
_publ_section_title
;
 Revealing the remarkable structural diversity of the alkali metal
 transfer agents of the trans-calix[2]benzene[2]pyrrolide ligand.
;
_journal_issue                   82
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              12199
_journal_page_last               12201
_journal_paper_doi               10.1039/c6cc07240b
_journal_volume                  52
_journal_year                    2016
_chemical_formula_moiety         'C40 H52 N2 Na2 O2'
_chemical_formula_sum            'C40 H52 N2 Na2 O2'
_chemical_formula_weight         638.81
_chemical_properties_physical
', Air-sensitive,Moisture-sensitive,Oxygen-sensitive'
_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_Hall           'C -2yc'
_space_group_name_H-M_alt        'C 1 c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2016-08-16 deposited with the CCDC.
2016-09-19 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90.7580(10)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   10.2275(2)
_cell_length_b                   35.0736(6)
_cell_length_c                   19.9910(3)
_cell_measurement_reflns_used    10733
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      72.9530
_cell_measurement_theta_min      4.5070
_cell_volume                     7170.4(2)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_collection
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_molecular_graphics    'SHELXLE (Hubschle, Sheldrick and Dittrich)'
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_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      123(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Oxford Diffraction Gemini S'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0228
_diffrn_reflns_av_unetI/netI     0.0321
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       12
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_diffrn_reflns_limit_l_max       23
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_diffrn_reflns_number            17946
_diffrn_reflns_point_group_measured_fraction_full 0.704
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_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         69.999
_diffrn_reflns_theta_min         6.360
_exptl_absorpt_coefficient_mu    0.766
_exptl_absorpt_correction_T_max  1.00000
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Empirical absorption correction using spherical harmonics,
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_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.183
_exptl_crystal_description       block
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_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.34
_exptl_crystal_size_min          0.26
_refine_diff_density_max         0.853
_refine_diff_density_min         -0.370
_refine_diff_density_rms         0.053
_refine_ls_abs_structure_details
;
 Flack x determined using 2388 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.06(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     933
_refine_ls_number_reflns         9491
_refine_ls_number_restraints     315
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0576
_refine_ls_R_factor_gt           0.0546
_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^)+(0.1089P)^2^+4.3876P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1509
_refine_ls_wR_factor_ref         0.1556
_reflns_Friedel_coverage         0.398
_reflns_Friedel_fraction_full    0.411
_reflns_Friedel_fraction_max     0.398
_reflns_number_gt                8953
_reflns_number_total             9491
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6cc07240b2.cif
_cod_data_source_block           ammf_g430smartweebox
_cod_depositor_comments
;

2024-03-12
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C80 H104 N4 Na4 O4'
_cod_original_formula_weight         1277.63
_cod_original_formula_moiety         'C80 H104 N4 Na4 O4'
_cod_original_formula_units_Z            4
_cod_original_sg_symbol_H-M      'C c'
_cod_database_code               7125160
_shelx_shelxl_version_number     2014/7
_shelx_res_checksum              30078