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_7122183
_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            'C44 H61 B I2 N3 O7 U'
_chemical_formula_weight         1246.59
_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
;
2018-06-27 deposited with the CCDC.
2018-08-15 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 107.307(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   20.142(3)
_cell_length_b                   9.6317(16)
_cell_length_c                   26.979(5)
_cell_measurement_reflns_used    9993
_cell_measurement_temperature    133(2)
_cell_measurement_theta_max      27.77
_cell_measurement_theta_min      2.23
_cell_volume                     4997.0(15)
_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 0.971
_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  0.0588
_diffrn_reflns_av_unetI/netI     0.0503
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.971
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            58739
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.971
_diffrn_reflns_theta_full        25.500
_diffrn_reflns_theta_max         28.343
_diffrn_reflns_theta_min         1.498
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    4.531
_exptl_absorpt_correction_T_max  0.4311
_exptl_absorpt_correction_T_min  0.3498
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker SADABS 2014/5'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.657
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    not_measured
_exptl_crystal_description       rectangle
_exptl_crystal_F_000             2420
_exptl_crystal_size_max          0.207
_exptl_crystal_size_mid          0.136
_exptl_crystal_size_min          0.121
_refine_diff_density_max         1.717
_refine_diff_density_min         -1.217
_refine_diff_density_rms         0.135
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     525
_refine_ls_number_reflns         12099
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.019
_refine_ls_R_factor_all          0.0528
_refine_ls_R_factor_gt           0.0346
_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^)+(0.0353P)^2^+1.5018P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0709
_refine_ls_wR_factor_ref         0.0766
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9551
_reflns_number_total             12099
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8cc05341c2.cif
_cod_data_source_block           dnh54
_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_original_cell_volume        4996.9(15)
_cod_database_code               7122183
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.454
_shelx_estimated_absorpt_t_max   0.610
_exptl_absorpt_special_details
; 
Reflections not merged 
60734 Corrected reflections written to file dnh54s.hkl 
Estimated minimum and maximum transmission:  0.3498  0.4311 
The ratio (0.8114) 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              9628
_shelx_fab_checksum              50246