Carbon monoxide coupling and functionalisation at a simple uranium coordination complex
Arnold, Polly L.; Turner, Zoë R.; Bellabarba, Ronan M.; Tooze, Robert P.; Chemical Science 2 (2011) 77–; doi:10.1039/c0sc00452a

data_1515664
_publ_section_title
;
 Carbon monoxide coupling and functionalisation at a simple uranium
 coordination complex
;
_journal_issue                   1
_journal_name_full               'Chemical Science'
_journal_page_first              77
_journal_paper_doi               10.1039/c0sc00452a
_journal_volume                  2
_journal_year                    2011
_chemical_formula_moiety         'C57 H162 N9 O3 Si18 U3'
_chemical_formula_sum            'C57 H162 N9 O3 Si18 U3'
_chemical_formula_weight         2241.67
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 103.691(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   30.0251(6)
_cell_length_b                   15.6531(3)
_cell_length_c                   22.4759(4)
_cell_measurement_reflns_used    20552
_cell_measurement_temperature    170(2)
_cell_measurement_theta_max      29.1301
_cell_measurement_theta_min      2.9477
_cell_volume                     10263.2(3)
_computing_cell_refinement
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET)
(compiled Jan 5 2010,16:28:46)
;
_computing_data_collection
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET)
(compiled Jan 5 2010,16:28:46)
;
_computing_data_reduction
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET)
(compiled Jan 5 2010,16:28:46)
;
_computing_molecular_graphics    'ORTEP-III (Farrugia, 2005)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR-92 (Giacovazzo, 1994)'
_diffrn_ambient_temperature      170(2)
_diffrn_detector_area_resol_mean 16.1042
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.860
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0324
_diffrn_reflns_av_sigmaI/netI    0.0872
_diffrn_reflns_limit_h_max       37
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            57493
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         2.95
_exptl_absorpt_coefficient_mu    4.970
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.81130
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET)
(compiled Jan 5 2010,16:28:46)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            gold
_exptl_crystal_density_diffrn    1.451
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             4476
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.14
_refine_diff_density_max         8.542
_refine_diff_density_min         -4.670
_refine_diff_density_rms         0.194
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.076
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     863
_refine_ls_number_reflns         23909
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.076
_refine_ls_R_factor_all          0.1118
_refine_ls_R_factor_gt           0.0654
_refine_ls_shift/su_max          0.012
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0905P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1640
_refine_ls_wR_factor_ref         0.1752
_reflns_number_gt                14064
_reflns_number_total             22833
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            c0sc00452a.txt
_cod_data_source_block           p10006_N3UOCHCROUN2andN3UOCCOUN3inasymunit
_cod_original_sg_symbol_H-M      P21/c
_cod_database_code               1515664