Synthesis of uranium-in-cryptand complexes.
Huh, Daniel N.; Windorff, Cory J.; Ziller, Joseph W.; Evans, William J.; Chemical communications (Cambridge, England) 54 (2018) 10272–10275; doi:10.1039/c8cc05341c

data_7122182
_publ_section_title
;
 Synthesis of uranium-in-cryptand complexes.
;
_journal_issue                   73
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              10272
_journal_page_last               10275
_journal_paper_doi               10.1039/c8cc05341c
_journal_volume                  54
_journal_year                    2018
_chemical_formula_sum            'C18 H38 I3 N2 O7 U'
_chemical_formula_weight         1013.23
_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
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2018-08-10 deposited with the CCDC.
2018-08-15 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 96.0099(13)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.8943(11)
_cell_length_b                   19.313(2)
_cell_length_c                   13.3229(14)
_cell_measurement_reflns_used    9851
_cell_measurement_temperature    133(2)
_cell_measurement_theta_max      28.65
_cell_measurement_theta_min      2.16
_cell_volume                     2787.8(5)
_computing_cell_refinement       'Bruker SAINT 8.34a, 2013'
_computing_data_collection       'Bruker APEX2 2014.11-0, 2014'
_computing_data_reduction        'Bruker SAINT 8.34a, 2013'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'Bruker SHELXTL 2014/4'
_diffrn_ambient_temperature      133(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker SMART APEX II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0494
_diffrn_reflns_av_unetI/netI     0.0362
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            31414
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.500
_diffrn_reflns_theta_max         27.103
_diffrn_reflns_theta_min         1.864
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    9.181
_exptl_absorpt_correction_T_max  0.4316
_exptl_absorpt_correction_T_min  0.3056
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker SADABS 2014/5'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    2.414
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    not_measured
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1868
_exptl_crystal_size_max          0.404
_exptl_crystal_size_mid          0.241
_exptl_crystal_size_min          0.154
_refine_diff_density_max         2.792
_refine_diff_density_min         -1.209
_refine_diff_density_rms         0.243
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.257
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     288
_refine_ls_number_reflns         6137
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.257
_refine_ls_R_factor_all          0.0523
_refine_ls_R_factor_gt           0.0474
_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^)+(0.0244P)^2^+46.0217P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1077
_refine_ls_wR_factor_ref         0.1096
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5617
_reflns_number_total             6137
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8cc05341c2.cif
_cod_data_source_block           cjw56
_cod_depositor_comments
;
The following automatic conversions were performed:

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

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

 Adding full bibliography for 7122180--7122183.cif.
;
_cod_database_code               7122182
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.119
_shelx_estimated_absorpt_t_max   0.332
_exptl_absorpt_special_details
;
Reflections not merged
33397 Corrected reflections written to file cjw56s.hkl
Estimated minimum and maximum transmission:  0.3056  0.4316
The ratio (0.7081) of these values is more reliable than their 
absolute values. Additional spherical absorption correction 
applied with mu*r =  0.6000. Lambda/2 correction factor = 0.00150
;
_shelx_res_checksum              479