Perrhenate and pertechnetate complexation by an azacryptand in nitric acid medium.
Thevenet, Alexiane; Marie, Cécile; Tamain, Christelle; Amendola, Valeria; Miljkovic, Ana; Guillaumont, Dominique; Boubals, Nathalie; Guilbaud, Philippe; Dalton transactions (Cambridge, England : 2003) 49 (2020) 1446–1455; doi:10.1039/c9dt04314d

data_7703665
_publ_section_title
;
 Perrhenate and pertechnetate complexation by an azacryptand in nitric
 acid medium.
;
_journal_issue                   5
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              1446
_journal_page_last               1455
_journal_paper_doi               10.1039/c9dt04314d
_journal_volume                  49
_journal_year                    2020
_chemical_formula_sum            'C36 H64 N11.5 O22.5 Re2.5'
_chemical_formula_weight         1483.48
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2019-09-02 deposited with the CCDC.	2020-01-09 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 107.4263(14)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.1970(9)
_cell_length_b                   16.7678(8)
_cell_length_c                   17.7700(9)
_cell_measurement_reflns_used    9985
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      27.6
_cell_measurement_theta_min      2.34
_cell_volume                     5173.2(4)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXL-2018/3 (Sheldrick, 2018)'
_diffrn_ambient_temperature      153(2)
_diffrn_measured_fraction_theta_full 0.972
_diffrn_measured_fraction_theta_max 0.928
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0217
_diffrn_reflns_av_unetI/netI     0.0324
_diffrn_reflns_Laue_measured_fraction_full 0.972
_diffrn_reflns_Laue_measured_fraction_max 0.928
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            31656
_diffrn_reflns_point_group_measured_fraction_full 0.972
_diffrn_reflns_point_group_measured_fraction_max 0.928
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.549
_diffrn_reflns_theta_min         1.173
_exptl_absorpt_coefficient_mu    5.928
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.905
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2912
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.080
_exptl_crystal_size_min          0.050
_exptl_transmission_factor_max   0.7456
_exptl_transmission_factor_min   0.6032
_refine_diff_density_max         3.282
_refine_diff_density_min         -1.223
_refine_diff_density_rms         0.136
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.961
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     759
_refine_ls_number_reflns         11088
_refine_ls_number_restraints     35
_refine_ls_restrained_S_all      0.968
_refine_ls_R_factor_all          0.0462
_refine_ls_R_factor_gt           0.0326
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0339P)^2^+35.8281P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0756
_refine_ls_wR_factor_ref         0.0821
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9257
_reflns_number_total             11088
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt04314d2.cif
_cod_data_source_block           CM_CT_Re_L_1
_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 7556 2019-12-06 15:28:31Z antanas 
;
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_original_formula_sum        'C36 H64 N11.50 O22.50 Re2.50'
_cod_database_code               7703665
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.589
_shelx_estimated_absorpt_t_max   0.756
_shelx_res_checksum              19925